CN112679950A - Preparation method of flexible carbon-carbon composite material - Google Patents
Preparation method of flexible carbon-carbon composite material Download PDFInfo
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- CN112679950A CN112679950A CN202011540869.7A CN202011540869A CN112679950A CN 112679950 A CN112679950 A CN 112679950A CN 202011540869 A CN202011540869 A CN 202011540869A CN 112679950 A CN112679950 A CN 112679950A
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Abstract
The invention discloses a preparation method of a flexible carbon-carbon composite material, and belongs to the field of carbon-carbon composite materials. The thermosetting resin and the carbon fiber cloth are used as raw materials, and the thermosetting resin is subjected to melting and cooling treatment to prepare a thermosetting resin adhesive film; after the obtained thermosetting resin adhesive film is laid on the surface of the carbon fiber cloth, hot-pressing compounding and curing operations are carried out to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material; and carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in an inert atmosphere to obtain the flexible carbon-carbon composite material. According to the invention, through reasonable preparation steps, the thermosetting resin and the carbon fiber braided fabric are carbonized after being subjected to hot pressing and compounding, and the flexible carbon-carbon composite material is successfully prepared by adopting a preparation method with a simple process. The preparation method has the advantages of short heat treatment time, no need of high-pressure heat treatment equipment and high production efficiency, and therefore, the industrial production can be conveniently realized.
Description
Technical Field
The invention relates to the field of carbon-carbon composite materials, in particular to a preparation method of a flexible carbon-carbon composite material.
Background
The carbon-carbon composite material has the characteristics of stable friction coefficient, wear resistance, high temperature resistance, high heat conductivity, excellent mechanical property and the like, is widely applied to the mechanical friction field of airplane brake pads, high-performance sports car brake pads and the like and the high-temperature equipment thermal field, but the existing carbon-carbon composite material belongs to a rigid material and cannot meet the requirements of the friction field and the like on flexible products, and a literature proposes to prepare the flexible carbon-carbon composite friction material by a vapor deposition method, but the method has low production efficiency and cannot be simply and conveniently applied to large-scale industrial production.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of a flexible carbon-carbon composite material. The preparation method solves the problems of high rigidity, complex preparation process and low efficiency of the existing carbon-carbon composite material product.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention discloses a preparation method of a flexible carbon-carbon composite material, which comprises the following steps:
step 1, preparing a thermosetting resin adhesive film; preparing thermosetting resin film by melting and coating thermosetting resin, and cooling the obtained thermosetting resin film to prepare thermosetting resin film;
step 2, after the obtained thermosetting resin adhesive film is laid on the surface of the carbon fiber cloth, hot-pressing compounding and curing operations are carried out to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material;
and 3, carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in an inert atmosphere to obtain the flexible carbon-carbon composite material.
Preferably, in step 1, the thermosetting resin is a high-carbon-residue-rate resin.
Further preferably, the high-carbon-residue-rate resin is any one of polyimide, bismaleimide, cyanate resin, benzoxazine, phenolic resin and epoxy resin or a modified resin thereof.
Preferably, in the step 1, the melting and heating temperature range of the thermosetting resin is 60 to 110 ℃.
Preferably, in the step 1, the obtained thermosetting resin film has an areal density of 6g/m2～300g/m2。
Preferably, in the step 2, the operation of thermal compression compounding and curing specifically includes: the compounding temperature is 60-110 ℃, the compounding time is 10-30 min, the compounding pressure is 0.1-0.3 MPa, the curing temperature is 130-260 ℃, the curing time is 10-60 min, and the curing pressure is 0.3-5 MPa.
Preferably, in the step 2, the carbon fiber cloth is polyacrylonitrile-based carbon fiber laid cloth or woven cloth, pitch-based carbon fiber laid cloth or woven cloth, or viscose-based carbon fiber laid cloth or woven cloth.
Preferably, in the step 2, the number of twists of the carbon fiber cloth is 0 to 200 twists/m, and the surface density is 20g/m2～1000g/m2。
Preferably, in the step 2), the weight ratio of the glue film to the total weight of the glue film and the carbon fiber cloth is 5-60%.
Preferably, in the step 3, the temperature of the carbonization treatment is 600-2900 ℃, and the heat preservation time of the carbonization treatment is 0-60 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of a flexible carbon-carbon composite material, which is characterized in that thermosetting resin and carbon fiber cloth which are conventional industrial production raw materials are used as raw materials, and through reasonable preparation steps, the thermosetting resin and the carbon fiber cloth are subjected to hot-pressing compounding and carbonization treatment, so that the flexible carbon-carbon composite material can be prepared. The preparation method has the advantages of simple process, short heat treatment time, no need of high-pressure heat treatment equipment, high production efficiency, no solvent and convenience for realizing industrial production. The invention adopts the method that the carbon fiber cloth and the thermosetting resin are subjected to hot-pressing compounding and then are subjected to heat treatment to prepare the carbon-carbon composite material, compared with the traditional carbon-carbon composite material which adopts a three-dimensional braided fabric as a reinforcement, the size in the thickness direction is obviously reduced, the thermosetting resin adhesive film is formed by melting the thermosetting resin, the obtained thermosetting resin adhesive film and the carbon fiber cloth are subjected to hot-pressing compounding and curing impregnation treatment and carbonization processes to form the low-density flexible carbon-carbon composite material, compared with the traditional carbon-carbon composite material, the density is reduced, but the flexible carbon-carbon composite material has the bendable and flexible functions which are not possessed by the traditional carbon-carbon composite material, compared with the flexible carbon-carbon composite material prepared by the existing vapor deposition process, the flexible carbon-carbon composite material can be stacked and placed for hot pressing and heat treatment in the hot pressing and heat treatment processes, the yield is, meanwhile, gas and organic solvent are not used, and the production process is easy to control.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to 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.
It is to be understood that the terms first, second and the like in the description and in the claims are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention discloses a preparation method of a flexible carbon-carbon composite material, which is realized by the following specific steps:
1) thermosetting resin adhesive film preparation
The thermosetting resin is any one of polyimide, bismaleimide, cyanate resin, benzoxazine, phenolic resin and epoxy resin or modified resin thereof.
Stirring and heating the thermosetting resin to a molten state, wherein the heating temperature is 60-110 ℃, the heating and stirring time is 30-120 min, the stirring speed is 100-500 r/min, and a thermosetting resin film with the surface density of 10-400 g/m is prepared on a coating machine2And (3) placing the prepared thermosetting resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 10-20 ℃, and the cooling time is 5-10 s, so as to prepare the thermosetting resin adhesive film.
2) Carbon fiber braided fabric and thermosetting resin adhesive film composite curing
Placing the prepared thermosetting resin adhesive film on the upper surface and the lower surface of the carbon fiber cloth for hot-pressing compounding and curing, wherein the hot-pressing compounding and curing operation specifically comprises the following steps: the compounding temperature is 60-110 ℃, the compounding time is 10-30 min, the compounding pressure is 0.1-0.3 MPa, the curing temperature is 130-260 ℃, the curing time is 10-60 min, and the curing pressure is 0.3-5 MPa;
the carbon fiber cloth with the thickness of 0.02 mm-1 mm has the cloth surface density of 20g/m2～2000g/m2The carbon fiber cloth can be in the form of non-woven cloth, plain woven cloth, twill woven cloth, satin woven cloth and the like.
The carbon fiber cloth is polyacrylonitrile-based carbon fiber laid cloth or woven cloth, pitch-based carbon fiber laid cloth or woven cloth, viscose-based carbon fiber laid cloth or woven cloth, and can include: polyacrylonitrile-based pre-oxidized fiber laid cloth and woven cloth, pitch-based pre-oxidized fiber laid cloth and woven cloth, viscose-based pre-oxidized fiber laid cloth and woven cloth, carbonized polyacrylonitrile-based carbon fiber laid cloth and woven cloth, pitch-based carbon fiber woven fabric or viscose-based carbon fiber laid cloth and woven cloth, polyacrylonitrile-based carbon fiber laid cloth and woven cloth woven by polyacrylonitrile carbon fiber, pitch-based carbon fiber and viscose-based carbon fiber, pitch-based carbon fiber laid cloth and woven cloth, or viscose-based carbon fiber laid cloth and woven cloth.
Wherein, the carbon fiber or the pre-oxidized fiber can be twisted, and the twisting number is 0-200 twist/m.
The thermosetting resin adhesive film accounts for 5-60% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
3) Carbonizing
Carbonizing the carbon fiber braided fabric/thermosetting resin composite material: and carbonizing the carbon fiber braided fabric/thermosetting resin composite material in a carbonization furnace under inert atmosphere to obtain the flexible carbon-carbon composite material.
The carbonization treatment temperature is 600-2900 ℃, the heating rate is 0.5-20 ℃/min, and the heat preservation time of the carbonization treatment is 0-60 min.
The invention provides a method for preparing a flexible carbon-carbon composite material by heat treatment after compounding carbon fiber cloth and thermosetting resin, which solves the problems of high rigidity and low production efficiency of the existing carbon-carbon composite material product.
The invention will be further illustrated with reference to specific examples:
the first embodiment is as follows:
(1) selecting polyacrylonitrile-based carbon fiber laid cloth with thickness of 0.02mm and surface density of 20g/m2。
Heating the bismaleimide resin to 110 ℃, stirring for 60min at constant temperature, wherein the stirring speed is 200 r/min; preparing resin film with surface density of 6g/m from resin on a film coating machine2And (3) placing the resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 15 ℃, and the cooling time is 5s, so as to obtain the thermosetting resin adhesive film.
(2) Respectively paving a layer of thermosetting resin adhesive film on each of the upper and lower sides of the polyacrylonitrile-based carbon fiber untwisted twill braided fabric, and placing the polyacrylonitrile-based carbon fiber untwisted twill braided fabric on a hot press for hot-pressing compounding and curing, wherein the compounding temperature is 110 ℃, the compounding time is 30min, the pressure is 0.1MPa, the curing temperature is 180 ℃, the curing time is 60min, and the curing pressure is 1.5MPa, so as to obtain the thermosetting resin adhesive film/carbon fiber cloth composite material; the thermosetting resin adhesive film accounts for 60% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
(3) Carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in a carbonization furnace in nitrogen atmosphere, wherein the heating rate is 20 ℃/min, the highest temperature is 2900 ℃, and the heat preservation time is 5min, so as to obtain the flexible carbon-carbon composite material.
Cutting a flexible carbon-carbon composite material with the size of 200 x 200, selecting any 200 x 200 plane, taking two parallel edges in the plane as stress points, and bending a sample into a circular tube shape by 20N force always perpendicular to the 200 x 200 plane, wherein the curvature of a circular ring of the cross section of the circular tube is 1000m-1。
Example two:
(1) selecting polyacrylonitrile-based carbon fiber plain woven cloth with thickness of 0.2mm, carbon fiber twisting number of 50 twists/m, and surface density of 200g/m2。
Heating the polyimide resin to 110 ℃, stirring for 60min at constant temperature, wherein the stirring speed is 200 r/min; preparing resin film with surface density of 50g/m from resin on a film coating machine2And (3) placing the resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 10 ℃, and the cooling time is 10s, so as to obtain the thermosetting resin adhesive film.
(2) Respectively paving a layer of thermosetting resin adhesive film on the upper side and the lower side of the polyacrylonitrile-based carbon fiber cloth, and placing the polyacrylonitrile-based carbon fiber cloth on a hot press for hot-pressing compounding and curing, wherein the compounding temperature is 110 ℃, the time is 30min, the pressure is 0.3MPa, the curing temperature is 260 ℃, the curing time is 60min, and the curing pressure is 1.5MPa to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material; the thermosetting resin adhesive film accounts for 50% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
(3) Carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in a carbonization furnace in nitrogen atmosphere, wherein the heating rate is 5 ℃/min, the highest temperature is 1000 ℃, and the heat preservation time is 0, so as to obtain the flexible carbon-carbon composite material.
Cutting a flexible carbon-carbon composite material with the size of 200 x 200, selecting any 200 x 200 plane, taking two parallel edges in the plane as stress points, bending a sample into a circular tube shape by a force of 20N which is always vertical to the 200 x 200 plane, wherein the cross section of the circular tube is a circular ring with the curvature of 62m-1。
Example three:
(1) selecting an asphalt-based carbon fiber untwisted plain woven fabric with the thickness of 0.4mm and the surface density of 400g/m2。
Heating the cyanic acid resin to 80 ℃, stirring for 50min at constant temperature, wherein the stirring speed is 100 r/min; preparing resin film with surface density of 40g/m from resin on a film coating machine2And (3) placing the resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 10 ℃, and the cooling time is 5s, so as to obtain the thermosetting resin adhesive film.
(2) Respectively paving a layer of thermosetting resin adhesive film on the upper side and the lower side of the polyacrylonitrile-based carbon fiber cloth, and placing the polyacrylonitrile-based carbon fiber cloth on a hot press for hot-pressing compounding and curing, wherein the compounding temperature is 90 ℃, the time is 30min, the pressure is 0.3MPa, the curing temperature is 180 ℃, the curing time is 60min, and the curing pressure is 1.5MPa, so as to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material; the thermosetting resin adhesive film accounts for 20% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
(3) Carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in a carbonization furnace in nitrogen atmosphere, wherein the heating rate is 0.5 ℃/min, the highest temperature is 800 ℃, and the heat preservation time is 30min, so as to obtain the flexible carbon-carbon composite material.
Cutting a flexible carbon-carbon composite material with the size of 200 x 200, selecting any 200 x 200 plane, taking two parallel edges in the plane as stress points, and bending the sample into an arch shape by 20N force always vertical to the 200 x 200 plane, wherein the curvature of the arc of the arch cross section is 18m-1。
Example four:
(1) selecting polyacrylonitrile-based carbon fiber untwisted twill woven cloth with the thickness of 0.4mm and the surface density of 400g/m2。
Heating benzoxazine resin to 80 ℃, stirring for 50min at constant temperature, and stirring speed of 100 r/min; preparing resin film with surface density of 10g/m from resin on a film coating machine2And (3) placing the resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 10 ℃, and the cooling time is 5s, so as to obtain the thermosetting resin adhesive film.
(2) Respectively paving a layer of thermosetting resin adhesive film on the upper side and the lower side of the polyacrylonitrile-based carbon fiber cloth, and placing the polyacrylonitrile-based carbon fiber cloth on a hot press for hot-pressing compounding and curing, wherein the compounding temperature is 80 ℃, the time is 30min, the pressure is 0.3MPa, the curing temperature is 150 ℃, the curing time is 30min, and the curing pressure is 5MPa, so as to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material; the thermosetting resin adhesive film accounts for 5% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
(3) Carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in a carbonization furnace in nitrogen atmosphere, wherein the heating rate is 0.5 ℃/min, the highest temperature is 600 ℃, and the heat preservation time is 60min, so as to obtain the flexible carbon-carbon composite material.
Cutting a flexible carbon-carbon composite material with the size of 200 x 200, selecting any 200 x 200 plane, taking two parallel edges in the plane as stress points, and bending the sample into an arch shape by using a force with the size of 20N which is always vertical to the 200 x 200 plane, wherein the curvature of the arc of the arch section is 20m-1。
Example five:
(1) selecting the carbon fiber woven cloth after carbonizing the polyacrylonitrile-based preoxidized fiber twisted plain woven cloth, wherein the twisting number of the preoxidized fiber is 200 twists/m, the thickness is 1mm, and the density of the carbon fiber woven cloth surface is 1000g/m2。
Heating phenolic resin to 60 ℃, stirring at constant temperature for 30min, wherein the stirring speed is 500 r/min; preparing resin into resin film with surface density of 300g/m on a film coating machine2And (3) placing the resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 10 ℃, and the cooling time is 5s, so as to obtain the thermosetting resin adhesive film.
(2) Respectively paving a layer of thermosetting resin adhesive film on the upper side and the lower side of the polyacrylonitrile-based carbon fiber cloth, and placing the polyacrylonitrile-based carbon fiber cloth on a hot press for hot-pressing compounding and curing, wherein the compounding temperature is 60 ℃, the time is 20min, the pressure is 0.3MPa, the curing temperature is 150 ℃, the curing time is 30min, and the curing pressure is 5MPa, so as to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material; the thermosetting resin adhesive film accounts for 60% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
(3) Carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in a carbonization furnace in nitrogen atmosphere, wherein the heating rate is 0.5 ℃/min, the highest temperature is 600 ℃, and the heat preservation time is 30min, so as to obtain the flexible carbon-carbon composite material.
Cutting out flexible carbon-carbon composite material with size of 200 × 200, selecting any 200 × 200 plane, and using two parallel edges in the planeAs a stress point, the sample was bent into an arch shape with a curvature of 5m in the arc of the arch cross section with a force of 20N always perpendicular to the 200X 200 plane-1。
Example six:
(1) selecting viscose-based carbon fiber untwisted twill woven cloth with the thickness of 0.2mm and the surface density of 200g/m2。
Heating the epoxy resin to 65 ℃, stirring for 30min at a constant temperature, wherein the stirring speed is 500 r/min; preparing resin film with surface density of 25g/m from resin on a film coating machine2And (3) placing the resin film on a cooling plate for cooling, wherein the temperature of the cooling plate is 20 ℃, and the cooling time is 8s, so as to obtain the thermosetting resin adhesive film.
(2) Respectively paving a layer of thermosetting resin adhesive film on the upper side and the lower side of the polyacrylonitrile-based carbon fiber cloth, and placing the polyacrylonitrile-based carbon fiber cloth on a hot press for hot-pressing compounding and curing, wherein the compounding temperature is 80 ℃, the compounding time is 10min, the pressure is 0.1MPa, the curing temperature is 130 ℃, the curing time is 10min, and the curing pressure is 0.3MPa, so as to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material; the thermosetting resin adhesive film accounts for 25% of the total weight of the thermosetting resin adhesive film and the carbon fiber braided fabric in the compounding process.
(3) Carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in a carbonization furnace in nitrogen atmosphere, wherein the heating rate is 5 ℃/min, the highest temperature is 2900 ℃, and the heat preservation time is 5min, so as to obtain the flexible carbon-carbon composite material.
Cutting a flexible carbon-carbon composite material with the size of 200 multiplied by 200, selecting any 200 multiplied by 200 plane, taking two parallel edges in the plane as stress points, bending a sample into a round pipe by 20N force always vertical to the 200 multiplied by 200 plane, wherein the curvature of a circular ring on the section of the round pipe is 64m-1。
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a flexible carbon-carbon composite material is characterized by comprising the following steps:
step 1, preparing a thermosetting resin adhesive film; preparing thermosetting resin film by melting and coating thermosetting resin, and cooling the obtained thermosetting resin film to prepare thermosetting resin film;
step 2, after the obtained thermosetting resin adhesive film is laid on the surface of the carbon fiber cloth, hot-pressing compounding and curing operations are carried out to obtain a thermosetting resin adhesive film/carbon fiber cloth composite material;
and 3, carbonizing the obtained thermosetting resin adhesive film/carbon fiber cloth composite material in an inert atmosphere to obtain the flexible carbon-carbon composite material.
2. The method for preparing a flexible carbon-carbon composite material according to claim 1, wherein in step 1, the thermosetting resin is a high-carbon-residue resin.
3. The method for preparing a flexible carbon-carbon composite material according to claim 2, wherein the high-carbon-residue-rate resin is any one of polyimide, bismaleimide, cyanate resin, benzoxazine, phenolic resin and epoxy resin or a modified resin thereof.
4. The method for preparing a flexible carbon-carbon composite material according to claim 1, wherein in the step 1, the melting and heating temperature of the thermosetting resin is in the range of 60 to 110 ℃.
5. The method for producing a flexible carbon-carbon composite material according to claim 1, wherein in the step 1, the obtained thermosetting resin film has an areal density of 6g/m2～300g/m2。
6. The method for preparing a flexible carbon-carbon composite material according to claim 1, wherein in the step 2, the hot-press compounding and curing operation specifically comprises: the compounding temperature is 60-110 ℃, the compounding time is 10-30 min, the compounding pressure is 0.1-0.3 MPa, the curing temperature is 130-260 ℃, the curing time is 10-60 min, and the curing pressure is 0.3-5 MPa.
7. The method for preparing a flexible carbon-carbon composite material according to claim 1, wherein in the step 2, the carbon fiber cloth is polyacrylonitrile-based carbon fiber laid cloth or woven cloth, pitch-based carbon fiber laid cloth or woven cloth, or viscose-based carbon fiber laid cloth or woven cloth.
8. The method for preparing a flexible carbon-carbon composite material according to claim 1, wherein in the step 2, the number of twists of the carbon fiber cloth is 0 to 200 twists/m, and the areal density is 20g/m2～1000g/m2。
9. The continuous preparation method of the flexible carbon-carbon composite material as claimed in claim 1, wherein in the step 2), the weight ratio of the glue film to the total weight of the glue film and the carbon fiber cloth is 5-60%.
10. The method for preparing the flexible carbon-carbon composite material according to claim 1, wherein in the step 3, the temperature of the carbonization treatment is 600 ℃ to 2900 ℃, and the heat preservation time of the carbonization treatment is 0min to 60 min.
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