CN109777087B - High-content carbon fiber reinforced nylon composite material and preparation method thereof - Google Patents
High-content carbon fiber reinforced nylon composite material and preparation method thereof Download PDFInfo
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Abstract
A preparation method of a high-content carbon fiber reinforced nylon composite material comprises the steps of dipping an impurity-free carbon fiber cloth in an alcohol-soluble nylon absolute ethyl alcohol solution to obtain a dipped carbon fiber cloth, taking out the dipped carbon fiber cloth, drying to remove water to obtain a dried carbon fiber cloth, selecting a plurality of pieces of the dried carbon fiber cloth and a plurality of pieces of anhydrous nylon non-woven fabrics, wherein the mass of the dried carbon fiber cloth accounts for 65% -80% of the sum of the mass of the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics, alternately stacking the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics to obtain a stacked body, putting the stacked body into a mold, and performing hot-press molding to obtain the composite material. The design not only has good combination of the carbon fiber and the resin interface, but also has good mechanical property of the obtained composite material, higher carbon fiber content and easy operation.
Description
Technical Field
The invention relates to a carbon fiber reinforced nylon composite material, belongs to the field of composite materials, and particularly relates to a high-content carbon fiber reinforced nylon composite material and a preparation method thereof.
Background
The carbon fiber has the characteristics of high specific strength and high specific modulus, and is a good reinforcing material. At present, the carbon fiber reinforced thermosetting composite material is mainly characterized in that thermosetting resin is uniformly dispersed among carbon fiber monofilaments in a vacuum introduction mode, but the price of carbon fiber is high, so that the composite material prepared by using the thermosetting resin cannot be recycled, and resource waste is caused.
Meanwhile, thermoplastic resin is adopted in the prior art, but the viscosity of the thermoplastic resin is high, so that the processing difficulty is increased, the interface bonding between the carbon fibers and the thermoplastic resin is poor, and particularly when the content of the carbon fibers is high, the interface bonding between the carbon fibers and the thermoplastic resin is poor, so that the development of the carbon fiber reinforced thermoplastic resin is greatly hindered.
In addition, the conventional carbon fiber reinforced nylon composite material has a carbon fiber content of 60% or less in many cases, and cannot sufficiently exhibit excellent mechanical properties of carbon fibers.
The information disclosed in this background section is only for enhancement of understanding of the general background of the patent application and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects and problems of poor interface bonding between carbon fiber and resin and low carbon fiber content in the prior art, and provides a high-content carbon fiber reinforced nylon composite material with good interface bonding between carbon fiber and resin and high carbon fiber content and a preparation method thereof.
In order to achieve the above purpose, the technical solution of the invention is as follows: a preparation method of a high-content carbon fiber reinforced nylon composite material; the preparation method comprises the following steps:
the first step is as follows: removing water in the nylon non-woven fabric to obtain an anhydrous nylon non-woven fabric, and simultaneously removing surface impurities of the carbon fiber cloth to obtain impurity-free carbon fiber cloth;
the second step is that: firstly, soaking the impurity-free carbon fiber cloth in an alcohol-soluble nylon absolute ethyl alcohol solution to obtain soaked carbon fiber cloth, then taking out the soaked carbon fiber cloth, and drying to remove water to obtain dried carbon fiber cloth;
the third step: selecting a plurality of pieces of the dried carbon fiber cloth and a plurality of anhydrous nylon non-woven fabrics, wherein the mass of the dried carbon fiber cloth accounts for 65% -80% of the sum of the mass of the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics, alternately stacking the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics to obtain a stacked body, then putting the stacked body into a mold, and performing hot-press molding to obtain the composite material.
The mass percentage concentration of the alcohol-soluble nylon absolute ethyl alcohol solution is 0.5% -3%.
And the soaking time of the impurity-free carbon fiber cloth in the alcohol-soluble nylon absolute ethyl alcohol solution is 8-16 h.
The hot-press forming comprises a hot-press stage, a first cooling stage and a second cooling stage which are sequentially carried out;
the hot pressing stage is as follows: hot pressing the laminated body in the mould from the upper direction and the lower direction;
the first cooling stage is as follows: pressurizing and cooling the laminated body in the mold;
the second cooling stage is as follows: cooling the laminate in the mold;
the second cooling stage has a greater cooling rate than the first cooling stage.
In the hot pressing stage: the processing temperature is 230-280 ℃, the processing pressure is 5-30 Mpa, and the dwell time is 20-40 min.
In the first cooling stage: cooling to 170-200 deg.C, cooling at 1-5 deg.C/min, and maintaining at 170-200 deg.C for 1-2 hr;
in the second cooling stage: cooling to room temperature at a rate of 20-30 deg.C/min.
The step of removing the surface impurities of the carbon fiber cloth is as follows: firstly, soaking the carbon fiber cloth in an acetone solution for 4-6 h, and then carrying out ultrasonic treatment for 10-30 min to remove impurities on the surface of the carbon fiber cloth.
The step of removing the water in the nylon non-woven fabric is as follows: putting the nylon non-woven fabric into an oven, setting the temperature to be 80 ℃, and then preserving the heat for 8-12 hours to remove the water in the nylon non-woven fabric.
The nylon non-woven fabric is nylon 6 non-woven fabric or nylon 66 non-woven fabric, and the mass per unit area of the nylon non-woven fabric is 40-120 g/m2。
A high-content carbon fiber reinforced nylon composite material is prepared by the preparation method of the high-content carbon fiber reinforced nylon composite material; in the composite material, each carbon fiber monofilament is soaked with nylon resin, and the nylon resin is obtained by melting anhydrous nylon non-woven fabrics during hot-press molding.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to a high-content carbon fiber reinforced nylon composite material and a preparation method thereof, wherein impurity-free carbon fiber cloth is firstly dipped in alcohol-soluble nylon absolute ethyl alcohol solution to obtain dipped carbon fiber cloth, then the dipped carbon fiber cloth is taken out and dried to obtain dried carbon fiber cloth, then a laminated body obtained by alternately laminating the dried carbon fiber cloth and the anhydrous nylon non-woven cloth is subjected to hot press molding to obtain the composite material, in the whole preparation process, the impurity-free carbon fiber cloth is dipped in the alcohol-soluble nylon absolute ethyl alcohol solution to ensure that alcohol-soluble nylon is attached to the surface of a carbon fiber monofilament so as to improve the number of surface active groups of the carbon fiber monofilament, the alcohol-soluble nylon can be crosslinked with a molten body of the nylon non-woven cloth during the hot press molding, the molten body of the nylon non-woven cloth can be fully infiltrated to the carbon fiber monofilament to form a good interface layer, thereby greatly improving the mechanical property of the carbon fiber reinforced nylon composite material, in addition, the infiltration mode can ensure that the tissue structure of the carbon fiber cloth is not damaged by the flowing of the nylon resin (molten mass of the nylon non-woven fabric), and further improves the mechanical property of the composite material. Therefore, the carbon fiber and resin interface combination is better, and the mechanical property of the manufactured composite material is better.
2. According to the high-content carbon fiber reinforced nylon composite material and the preparation method thereof, the composite material is obtained by hot-press molding of a laminated body obtained by alternately laminating dried carbon fiber cloth and anhydrous nylon non-woven fabric, wherein the mass of the dried carbon fiber cloth accounts for 65% -80% of the sum of the mass of the dried carbon fiber cloth and the anhydrous nylon non-woven fabric, and the design can ensure that the finally obtained composite material contains carbon fibers with larger mass, so that the excellent mechanical property of the carbon fibers is fully exerted, and the mechanical property of the obtained composite material is improved. Therefore, the carbon fiber content in the invention is higher, and the mechanical property of the prepared composite material is better.
3. According to the high-carbon-fiber-content reinforced nylon composite material and the preparation method thereof, hot press forming of the laminated body is preferably performed in sequence through a hot press stage, a first cooling stage and a second cooling stage, wherein the cooling rate of the second cooling stage is higher than that of the first cooling stage. Therefore, the composite material prepared by the method has good mechanical property and high working efficiency.
4. According to the high-content carbon fiber reinforced nylon composite material and the preparation method thereof, the hot-pressed laminated body is composed of the dried carbon fiber cloth and the anhydrous nylon non-woven fabric, wherein the dried carbon fiber cloth and the anhydrous nylon non-woven fabric do not contain water, and the design can avoid the defects that the inside of the material is hollow and the like due to water evaporation in the hot-press molding process of the material. Therefore, the hot-press forming effect of the invention is better.
5. The invention relates to a high-content carbon fiber reinforced nylon composite material and a preparation method thereof, which mainly comprise a step of dipping impurity-free carbon fiber cloth in an alcohol-soluble nylon absolute ethyl alcohol solution and a step of hot-press molding of a laminated body, wherein the steps are fewer, the front-back connectivity is better, the preparation method is easy to operate, the pressure, the temperature and the time during hot-press molding can be controlled, and the product dimension stability is better. Therefore, the invention is not only easy to operate, but also has strong product controllability.
Drawings
FIG. 1 is a schematic view of the structure of a laminate in the present invention.
In the figure: the blank square refers to an anhydrous nylon non-woven fabric, and the grid square refers to a dried carbon fiber cloth.
Detailed Description
The present invention will be described in further detail with reference to the following description and embodiments in conjunction with the accompanying drawings.
Referring to fig. 1, a preparation method of a high-content carbon fiber reinforced nylon composite material comprises the following steps:
the first step is as follows: removing water in the nylon non-woven fabric to obtain an anhydrous nylon non-woven fabric, and simultaneously removing surface impurities of the carbon fiber cloth to obtain impurity-free carbon fiber cloth;
the second step is that: firstly, soaking the impurity-free carbon fiber cloth in an alcohol-soluble nylon absolute ethyl alcohol solution to obtain soaked carbon fiber cloth, then taking out the soaked carbon fiber cloth, and drying to remove water to obtain dried carbon fiber cloth;
the third step: selecting a plurality of pieces of the dried carbon fiber cloth and a plurality of anhydrous nylon non-woven fabrics, wherein the mass of the dried carbon fiber cloth accounts for 65% -80% of the sum of the mass of the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics, alternately stacking the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics to obtain a stacked body, then putting the stacked body into a mold, and performing hot-press molding to obtain the composite material.
The mass percentage concentration of the alcohol-soluble nylon absolute ethyl alcohol solution is 0.5% -3%.
And the soaking time of the impurity-free carbon fiber cloth in the alcohol-soluble nylon absolute ethyl alcohol solution is 8-16 h.
The hot-press forming comprises a hot-press stage, a first cooling stage and a second cooling stage which are sequentially carried out;
the hot pressing stage is as follows: hot pressing the laminated body in the mould from the upper direction and the lower direction;
the first cooling stage is as follows: pressurizing and cooling the laminated body in the mold;
the second cooling stage is as follows: cooling the laminate in the mold;
the second cooling stage has a greater cooling rate than the first cooling stage.
In the hot pressing stage: the processing temperature is 230-280 ℃, the processing pressure is 5-30 Mpa, and the dwell time is 20-40 min.
In the first cooling stage: cooling to 170-200 deg.C, cooling at 1-5 deg.C/min, and maintaining at 170-200 deg.C for 1-2 hr;
in the second cooling stage: cooling to room temperature at a rate of 20-30 deg.C/min.
The step of removing the surface impurities of the carbon fiber cloth is as follows: firstly, soaking the carbon fiber cloth in an acetone solution for 4-6 h, and then carrying out ultrasonic treatment for 10-30 min to remove impurities on the surface of the carbon fiber cloth.
The step of removing the water in the nylon non-woven fabric is as follows: putting the nylon non-woven fabric into an oven, setting the temperature to be 80 ℃, and then preserving the heat for 8-12 hours to remove the water in the nylon non-woven fabric.
The nylon non-woven fabric is nylon 6 non-woven fabric or nylon 66 non-woven fabric, and the mass per unit area of the nylon non-woven fabric is 40-120 g/m2。
A high-content carbon fiber reinforced nylon composite material is prepared by the preparation method of the high-content carbon fiber reinforced nylon composite material; in the composite material, each carbon fiber monofilament is soaked with nylon resin, and the nylon resin is obtained by melting anhydrous nylon non-woven fabrics during hot-press molding.
The principle of the invention is illustrated as follows:
in the prior art, when a carbon fiber fabric is used as a reinforcement, carbon fibers are arranged compactly, nylon resin cannot fully infiltrate carbon fiber monofilaments, meanwhile, the surface functional groups of the carbon fibers are few, the interface bonding effect of the fibers and the resin is poor, and particularly, when the content of the carbon fibers is high, the defect is more obvious, aiming at the defect, the invention provides a preparation method of a high-content carbon fiber reinforced nylon composite material, which can not only ensure that the content of the carbon fibers is higher than 65%, but also can remarkably improve the mechanical property of the composite material, and the main technical scheme is as follows: the carbon fiber cloth is pretreated (impregnated) firstly, so that part of nylon resin (namely alcohol-soluble nylon) is attached to the surface of a carbon fiber monofilament, the number of active groups on the surface of the carbon fiber monofilament is increased, the alcohol-soluble nylon can be crosslinked with a molten body of the nylon non-woven fabric during hot-press forming, the nylon resin is fully soaked into the carbon fiber monofilament in the hot-press process, a good interface layer is formed, and the mechanical property of the composite material is obviously improved. Meanwhile, the infiltration process can also protect the organization structure of the carbon fiber cloth, so that the carbon fiber cloth cannot be damaged due to the flowing of resin, and the mechanical property of the carbon fiber reinforced nylon composite material is greatly improved.
The carbon fiber cloth is preferably carbon fiber plain cloth, twill cloth, satin cloth or unidirectional cloth, and the fiber diameter is 5-10 μm.
The surface impurities of the carbon fiber cloth mainly refer to sizing agents (mainly epoxy slurry) and dust on the surface of the carbon fiber cloth, and the epoxy slurry is not beneficial to nylon resin to soak carbon fibers in the hot pressing process.
In the laminated body of the present invention, a layer of dried carbon fiber cloth is disposed between two adjacent layers of anhydrous nylon nonwoven fabrics, and a layer of anhydrous nylon nonwoven fabric is disposed between two adjacent layers of dried carbon fiber cloth, and the specific structure can be seen in fig. 1, and in addition, the expression "a plurality of pieces of dried carbon fiber cloth and a plurality of pieces of anhydrous nylon nonwoven fabrics" in the present invention means: the number of the carbon fiber cloth and the anhydrous nylon non-woven cloth after drying are natural numbers.
Example 1:
a preparation method of a high-content carbon fiber reinforced nylon composite material comprises the following steps:
the first step is as follows: removing water in the nylon non-woven fabric to obtain an anhydrous nylon non-woven fabric, and simultaneously removing surface impurities of the carbon fiber cloth to obtain impurity-free carbon fiber cloth;
the second step is that: firstly, soaking the impurity-free carbon fiber cloth in an alcohol-soluble nylon absolute ethyl alcohol solution to obtain soaked carbon fiber cloth, then taking out the soaked carbon fiber cloth, and drying to remove water to obtain dried carbon fiber cloth; preferably, the mass percent concentration of the alcohol-soluble nylon absolute ethyl alcohol solution is 0.5% -3%; preferably, the soaking time of the non-impurity carbon fiber cloth in the alcohol-soluble nylon absolute ethyl alcohol solution is 8-16 h;
the third step: selecting a plurality of pieces of the dried carbon fiber cloth and a plurality of anhydrous nylon non-woven fabrics, wherein the mass of the dried carbon fiber cloth accounts for 65% -80% of the sum of the mass of the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics, alternately stacking the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics to obtain a stacked body, then putting the stacked body into a mold, and performing hot-press molding to obtain the composite material.
A high-content carbon fiber reinforced nylon composite material is prepared by the preparation method of the high-content carbon fiber reinforced nylon composite material; in the composite material, each carbon fiber monofilament is soaked with nylon resin, and the nylon resin is obtained by melting anhydrous nylon non-woven fabrics during hot-press molding.
Example 2:
the basic contents are the same as example 1, except that:
the hot-press forming comprises a hot-press stage, a first cooling stage and a second cooling stage which are sequentially carried out;
the hot pressing stage is as follows: hot pressing the laminated body in the mould from the upper direction and the lower direction;
the first cooling stage is as follows: pressurizing and cooling the laminated body in the mold;
the second cooling stage is as follows: cooling the laminate in the mold;
the second cooling stage has a greater cooling rate than the first cooling stage.
Example 3:
the basic content is the same as that of the embodiment 2, except that:
in the hot pressing stage: the processing temperature is 230-280 ℃, the processing pressure is 5-30 Mpa, and the dwell time is 20-40 min.
In the first cooling stage: cooling to 170-200 deg.C, cooling at 1-5 deg.C/min, and maintaining at 170-200 deg.C for 1-2 hr; in the second cooling stage: cooling to room temperature at a rate of 20-30 deg.C/min.
Example 4:
the basic contents are the same as example 1, except that:
the step of removing the surface impurities of the carbon fiber cloth is as follows: firstly, soaking the carbon fiber cloth in an acetone solution for 4-6 h, and then carrying out ultrasonic treatment for 10-30 min to remove impurities on the surface of the carbon fiber cloth.
The step of removing the water in the nylon non-woven fabric is as follows: putting the nylon non-woven fabric into an oven, setting the temperature to be 80 ℃, and then preserving the heat for 8-12 hours to remove the water in the nylon non-woven fabric.
Example 5:
the basic contents are the same as example 1, except that:
the nylon non-woven fabric is nylon 6 non-woven fabric or nylon 66 non-woven fabric, and the mass per unit area of the nylon non-woven fabric is 40-120 g/m2。
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above embodiment, but equivalent modifications or changes made by those skilled in the art according to the present disclosure should be included in the scope of the present invention.
Claims (8)
1. A preparation method of a high-content carbon fiber reinforced nylon composite material is characterized by comprising the following steps: the preparation method comprises the following steps:
the first step is as follows: removing water in the nylon non-woven fabric to obtain an anhydrous nylon non-woven fabric, and simultaneously removing surface impurities of the carbon fiber cloth to obtain impurity-free carbon fiber cloth;
the second step is that: firstly, soaking the impurity-free carbon fiber cloth in an alcohol-soluble nylon absolute ethyl alcohol solution to obtain soaked carbon fiber cloth, then taking out the soaked carbon fiber cloth, and drying to remove water to obtain dried carbon fiber cloth;
the third step: selecting a plurality of pieces of dried carbon fiber cloth and a plurality of anhydrous nylon non-woven fabrics, wherein the mass of the dried carbon fiber cloth accounts for 65% -80% of the sum of the mass of the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics, alternately stacking the dried carbon fiber cloth and the anhydrous nylon non-woven fabrics to obtain a stacked body, putting the stacked body into a mold, and performing hot-press molding to obtain the composite material;
the nylon non-woven fabric is nylon 6 non-woven fabric or nylon 66 non-woven fabric, and the mass per unit area of the nylon non-woven fabric is 40-120 g/m2；
The hot-press forming comprises a hot-press stage, a first cooling stage and a second cooling stage which are sequentially carried out;
the hot pressing stage is as follows: hot pressing the laminated body in the mould from the upper direction and the lower direction;
the first cooling stage is as follows: pressurizing and cooling the laminated body in the mold;
the second cooling stage is as follows: cooling the laminate in the mold;
the second cooling stage has a greater cooling rate than the first cooling stage.
2. The preparation method of the high-carbon-fiber-reinforced nylon composite material as claimed in claim 1, wherein the preparation method comprises the following steps: the mass percentage concentration of the alcohol-soluble nylon absolute ethyl alcohol solution is 0.5% -3%.
3. The method for preparing the high-carbon-fiber-reinforced nylon composite material according to claim 1 or 2, wherein the method comprises the following steps: and the soaking time of the impurity-free carbon fiber cloth in the alcohol-soluble nylon absolute ethyl alcohol solution is 8-16 h.
4. The method for preparing the high-carbon-fiber-reinforced nylon composite material according to claim 1 or 2, wherein the method comprises the following steps: in the hot pressing stage: the processing temperature is 230-280 ℃, the processing pressure is 5-30 Mpa, and the dwell time is 20-40 min.
5. The method for preparing the high-carbon-fiber-reinforced nylon composite material according to claim 1 or 2, wherein the method comprises the following steps:
in the first cooling stage: cooling to 170-200 deg.C, cooling at 1-5 deg.C/min, and maintaining at 170-200 deg.C for 1-2 hr;
in the second cooling stage: cooling to room temperature at a rate of 20-30 deg.C/min.
6. The method for preparing the high-carbon-fiber-reinforced nylon composite material according to claim 1 or 2, wherein the method comprises the following steps: the step of removing the surface impurities of the carbon fiber cloth is as follows: firstly, soaking the carbon fiber cloth in an acetone solution for 4-6 h, and then carrying out ultrasonic treatment for 10-30 min to remove impurities on the surface of the carbon fiber cloth.
7. The method for preparing the high-carbon-fiber-reinforced nylon composite material according to claim 1 or 2, wherein the method comprises the following steps: the step of removing the water in the nylon non-woven fabric is as follows: putting the nylon non-woven fabric into an oven, setting the temperature to be 80 ℃, and then preserving the heat for 8-12 hours to remove the water in the nylon non-woven fabric.
8. The high-content carbon fiber reinforced nylon composite material is characterized in that: the composite material is prepared by adopting the preparation method of the high-content carbon fiber reinforced nylon composite material in the claim 1 or 2; in the composite material, each carbon fiber monofilament is soaked with nylon resin, and the nylon resin is obtained by melting anhydrous nylon non-woven fabrics during hot-press molding.
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| JPS58152049A (en) * | 1982-03-08 | 1983-09-09 | Mitsubishi Rayon Co Ltd | Composite material of carbon fiber reinforced polyamide resin |
| CN102173153A (en) * | 2010-12-13 | 2011-09-07 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of fiber reinforced composite material |
| JP2015030272A (en) * | 2013-08-06 | 2015-02-16 | Art&Tech株式会社 | Carbon fiber-containing nonwoven fabric structure and laminate structure of the same and method for producing them |
| CN207207293U (en) * | 2017-07-21 | 2018-04-10 | 吉林大学 | Carbon fiber reinforced polymer-based composite board |
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| JPS58152049A (en) * | 1982-03-08 | 1983-09-09 | Mitsubishi Rayon Co Ltd | Composite material of carbon fiber reinforced polyamide resin |
| CN102173153A (en) * | 2010-12-13 | 2011-09-07 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of fiber reinforced composite material |
| JP2015030272A (en) * | 2013-08-06 | 2015-02-16 | Art&Tech株式会社 | Carbon fiber-containing nonwoven fabric structure and laminate structure of the same and method for producing them |
| CN207207293U (en) * | 2017-07-21 | 2018-04-10 | 吉林大学 | Carbon fiber reinforced polymer-based composite board |
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