CN111169031B - Method for improving interlayer bonding strength of winding-formed carbon/carbon composite material - Google Patents
Method for improving interlayer bonding strength of winding-formed carbon/carbon composite material Download PDFInfo
- Publication number
- CN111169031B CN111169031B CN201911422008.6A CN201911422008A CN111169031B CN 111169031 B CN111169031 B CN 111169031B CN 201911422008 A CN201911422008 A CN 201911422008A CN 111169031 B CN111169031 B CN 111169031B
- Authority
- CN
- China
- Prior art keywords
- carbon
- winding
- resin
- composite material
- treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/32—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core on a rotating mould, former or core
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/38—Automated lay-up, e.g. using robots, laying filaments according to predetermined patterns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
Abstract
The invention discloses a method for improving interlayer bonding strength of a winding-formed carbon/carbon composite material, which comprises the following steps: firstly, selecting a core mould to clean, then laying demolding cloth, brushing a demolding agent, and then laying a soft temperature-resistant material; winding continuous carbon fibers pre-impregnated with resin on a core mold for laying a soft temperature-resistant material to form a fiber layer with glue, laying a net tire and needling, and forming a winding-needling piece on the core mold; curing and demolding the winding-needling piece, and removing the soft temperature-resistant material to obtain a cured piece; fourthly, carbonizing the solidified part to obtain a carbonized part; fifthly, performing high-temperature purification treatment on the carbonized part; and sixthly, processing the carbonized part subjected to high-temperature purification treatment by a machine to obtain the winding formed carbon/carbon composite material. According to the invention, the net tire is laid in the fiber layer with the adhesive, and the carbon fiber is introduced in the radial direction in combination with the needling treatment, so that the forming-compact integration of the winding process is realized, and the interlayer bonding strength of the winding formed carbon/carbon composite material is improved.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a method for improving interlayer bonding strength of a winding-formed carbon/carbon composite material.
Background
The winding forming technology of the composite material becomes an important process for processing the composite material, the winding forming can give full play to the component material nature of the composite material, the laying direction of the fiber reinforced material is accurate, the fiber volume content is high, and the strength exertion rate is good. Therefore, the carbon/carbon composite material product prepared by winding molding can maintain the continuous laying quality of the fibers and is beneficial to improving the hoop tensile property of the product. However, the winding formed carbon/carbon composite material product is only combined by the matrix material between the fiber reinforced materials, and the defects of layering, bulging and yarn falling are easily caused due to weak interlayer bonding strength in the preparation and application processes, so that the application effect of the winding formed carbon/carbon composite material product is greatly influenced.
The patent with the application number of 201280038583.6 discloses a method for improving the interlayer bonding strength of a winding forming composite material, which realizes the improvement of the interlayer bonding strength by inlaying the interlayer fibers through the change of winding angles of different layers; in the method, in order to inlay the fibers, the winding angle needs to be specially designed, so that the structural designability of the material is limited. The patent with the application number of 201310314805.9 discloses a forming method of a winding-formed carbon nanotube reinforced composite material, which effectively enhances the mechanical strength in the surface and between layers of the carbon nanotube by introducing the carbon nanotube in the winding forming process; but the method adopts the carbon nano tube to carry out in-plane and interlayer reinforcement, thereby improving the cost of raw materials. The patent with application number 201310301505.7 adopts a method of interlacing a plurality of long fiber layers and short fiber layers, and the interlayer bonding strength is high, so that the integral strength and rigidity of the glass fiber reinforced plastic pipe are strong. The technology realizes interlayer reinforcement by staggering a plurality of long fiber layers and short fiber layers, and the interlayer reinforcement effect is limited as can be seen from the principle that the interaction between the long fiber layers and the short fiber layers is difficult to be obviously improved only by simple alternate laying.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for improving interlayer bonding strength of a winding formed carbon/carbon composite material, aiming at the defects of the prior art. According to the method, the net tire is laid in the fiber layer with the adhesive, and the carbon fiber is introduced in the radial direction by combining a needling treatment process, so that the forming-compacting integration of the winding process is realized, the interlayer bonding strength of the wound and formed carbon/carbon composite material is obviously improved, the interlayer bonding strength of the finally obtained wound and formed carbon/carbon composite material is not lower than 10MPa, and the obvious defects of layering, bulging and yarn falling are avoided.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for improving interlayer bonding strength of a winding-formed carbon/carbon composite material is characterized by comprising the following steps:
step one, core mould preparation: selecting a core mould with the outer surface structure and the size similar to those of the inner surface structure and the size of the target product carbon/carbon composite material, assembling, cleaning the outer surface of the assembled core mould, laying demolding cloth on the outer surface of the cleaned core mould, brushing a demolding agent on the outer surface of the core mould, and laying a soft temperature-resistant material; the outer diameter of the core mold is 10 mm-60 mm smaller than the inner diameter of the target product carbon/carbon composite material;
step two, continuously winding the tape adhesive and performing needle punching forming: winding continuous carbon fibers pre-impregnated with resin on the outer surface of the core mold laid with the soft temperature-resistant material in the first step by using a winding machine to form a fiber layer with glue, laying a net tire on the fiber layer with glue formed by winding after winding a single layer or multiple layers in the winding process, and carrying out needling treatment on the net tire and the fiber layer with glue at the lower layer of the net tire to form a winding-needling piece with a quasi-three-way structure on the core mold; the thickness of the winding-needling piece of the quasi-three-way structure is not less than that of the target product carbon/carbon composite material;
step three, curing treatment: placing the winding-needling piece formed on the core mold in the second step into a curing furnace for curing treatment, then demolding and removing the soft temperature-resistant material to obtain a cured piece with a quasi-three-dimensional structure; the density of the quasi-three-dimensional structure solidified piece is 1.30g/cm3～1.50g/cm3；
Step four, carbonizing treatment: placing the quasi-three-dimensional structure solidified piece obtained in the third step in a carbonization furnace, and carrying out carbonization treatment under the protection of nitrogen or argon atmosphere and at the temperature of 850-1200 ℃ to obtain a quasi-three-dimensional structure carbonized piece; the density of the carbonized part with the quasi-three-dimensional structure is 1.00g/cm3～1.40g/cm3The interlayer bonding strength is not less than 8MPa, and obvious defects of layering, bulging and yarn falling are avoided;
step five, high-temperature treatment: carrying out high-temperature purification treatment on the carbonized part with the quasi-three-dimensional structure obtained in the fifth step at the temperature of 2000-2500 ℃;
step six, machining: machining the carbonized part subjected to high-temperature purification treatment in the sixth step to obtain a winding formed carbon/carbon composite material; the interlayer bonding strength of the winding forming carbon/carbon composite material is not less than 10MPa, and obvious defects of layering, bulging and yarn falling are avoided.
The method for improving the interlayer bonding strength of the winding-molded carbon/carbon composite material is characterized in that the core mold in the first step is made of metal or graphite. The core mold made of the material can resist the temperature of a subsequent curing process, does not react with continuous carbon fibers impregnated with resin in advance, is easy to process and form, is beneficial to smooth preparation of the winding-formed carbon/carbon composite material, is convenient to demould, and enlarges the preparation range of the winding-formed carbon/carbon composite material.
The method for improving the interlayer bonding strength of the winding-formed carbon/carbon composite material is characterized in that in the step one, the soft temperature-resistant material is one or more than two of a carbon felt, a carbon cloth, a carbon fiber net tire, graphite paper and a ceramic fiber felt, and the laying thickness of the soft temperature-resistant material is 5-30 mm. The optimized soft temperature-resistant material has good temperature resistance, can bear the temperature of the subsequent curing process, does not have obvious reaction and deformation, does not react with the product, is favorable for ensuring the dimensional accuracy of the wound and molded carbon/carbon composite material and ensures the stable structure and performance of the product; when the laying thickness of the soft temperature-resistant material is 5-30 mm, the pricking pin can be protected from being damaged in the process of needling, and continuous needling is facilitated.
The method for improving the interlayer bonding strength of the winding-molded carbon/carbon composite material is characterized in that in the first step, the soft temperature-resistant material is soaked by resin and then paved, or the soft temperature-resistant material is paved and then brushed or impregnated by resin, wherein the resin is phenolic resin or furfuryl ketone resin, and the curing temperature of the resin is not higher than that of the resin adopted by the continuous carbon fiber which is soaked in the resin in advance in the second step. The soft temperature-resistant material is pre-impregnated with resin or spread and then brushed or impregnated with resin, so that the internal resin with the adhesive fiber layer can be prevented from migrating to the soft temperature-resistant material layer, the gel content of a solidified part and the uniformity of the resin in the solidified part can be improved, and the density and the stability of a product obtained after carbonization can be improved.
The method for improving the interlayer bonding strength of the winding-formed carbon/carbon composite material is characterized in that in the step two, the continuous carbon fiber pre-impregnated with the resin is made of one or more of viscose fiber-based carbon fiber, polyacrylonitrile fiber-based carbon fiber and pitch fiber-based carbon fiber, the filament bundle of the continuous carbon fiber pre-impregnated with the resin is 1.5-24K, the net body is a thin felt made of chopped carbon fiber, and the surface density of the net body is 20g/m2～300g/m2. The preparation of carbon/carbon composite materials with different purposes is met by adopting the preferable materials, the carbon/carbon composite materials comprise structural parts and functional parts, and the combination of different types of carbon fibers is used, so that the carbon/carbon composite materials are beneficial to obtaining larger design and application range; the optimized filament bundle is 1.5K-24K and the source of the net tire, simultaneously can meet the preparation process and performance requirements of the carbon/carbon composite material, and the optimized net tire surface density is 20g/m2～300g/m2The requirement of interlaminar reinforcing effect in the needling process is met.
The method for improving the interlayer bonding strength of the winding-molded carbon/carbon composite material is characterized in that in the second step, the winding is dry winding, semi-dry winding or wet winding; the resin glue solution adopted by the continuous carbon fiber pre-impregnated with the resin is a thermosetting resin glue solution with a carbon residue rate of not less than 45%, and the thermosetting resin glue solution is an ethanol solution of furfuryl ketone resin or phenolic resin; the winding mode is that the hoop and the spiral are alternately wound, wherein the hoop winding angle is 85-89 degrees, and the spiral winding angle is 20-85 degrees. The carbon/carbon composite material prepared by the optimized winding method meets different requirements on a preparation device, preparation efficiency and process cost; after the winding piece obtained by the optimized glue solution is subjected to curing and carbonization treatment, the density of the carbonized piece with the quasi-three-dimensional structure is 1.00g/cm3～1.40g/cm3(ii) a The adoption of the optimized winding mode and the winding angle is beneficial to obtaining carbon/carbon composite with different structural performance designsA material.
The method for improving the interlayer bonding strength of the winding-formed carbon/carbon composite material is characterized in that in the process of laying the net tires in the step two, the net tires with the same width as the length of the core mold and the same length as the wound core mold circumference before laying the net tires are uniformly laid on the straight tube section of the core mold, the net tires which are cut into a fan shape and have the same area as the head sealing section are laid on the head sealing section of the core mold, the distance between the adjacent net tires in the same layer is not more than 0.2mm, and the gaps formed by laying the net tires in the adjacent layers are staggered. By implementing the net tire laying process and parameters, a net tire laying layer which is uniformly and tightly laid can be obtained, and the needling effect can be favorably exerted; meanwhile, the spacing and the position of the net tire laying gap are limited, so that the factor of weakening the strength of the product is avoided.
The method for improving the interlayer bonding strength of the winding-formed carbon/carbon composite material is characterized in that in the step two, the needling depth of the needling treatment is 1-10 mm, the needling frequency is 1-5 layers/time, and the needling density is 5 needles/cm2About 50 needles/cm2. The optimal needling treatment process and parameters can effectively connect different winding layers through radial arrangement of short fibers in the net tire, so that the effect of improving the interlayer bonding strength is achieved.
The method for improving the interlayer bonding strength of the winding-formed carbon/carbon composite material is characterized in that after the needling treatment in the step two, resin is brushed on the net body, resin powder or asphalt powder is sprayed on the net body, and the resin powder are the same as resin in resin glue solution adopted by continuous carbon fibers which are soaked in the resin in advance. Through the optimized net tire treatment process, the rubber content in the net tire is improved, so that the density of the carbonized part with the quasi-three-way structure is improved, and the density of the carbonized part with the quasi-three-way structure can meet 1.00g/cm3～1.40g/cm3The index requirements of (1).
The method for improving the interlayer bonding strength of the winding-molded carbon/carbon composite material is characterized in that the curing treatment in the step three is a rotation curing treatment, and the rotation speed adopted by the rotation curing treatment is 1-60 revolutions per minute. By adopting the optimized curing treatment mode, uneven distribution of resin in a curing part and reduction of product stability caused by migration of the resin due to gravity in the curing process can be effectively avoided; the preferred rotation rate avoids uneven distribution inside the cured part and reduced product stability due to resin migration toward the outer wall by centrifugal force when the rotation rate is too fast.
The method for improving the interlayer bonding strength of the winding-molded carbon/carbon composite material is characterized in that when the density of the carbonized curing piece is less than that of the target product carbon/carbon composite material in the step four, the carbonized curing piece is densified, and the specific process is as follows: impregnating and curing the carbonized curing piece by using furfuryl ketone resin or pitch, then carbonizing to finish single densification, and repeating the single densification process of impregnation, curing and carbonization until the density of the densified curing piece is 1.00g/cm3～1.40g/cm3The solidified part after densification treatment is a carbonized part with a quasi-three-dimensional structure; when the density increase of the single densification is less than 0.3g/cm3When in use, the solidified piece after single densification is subjected to tapping treatment at 1800-2500 ℃, and then the single densification process is repeated; the infiltration pressure is 1.0MPa to 3.0MPa, the curing temperature is 160 ℃ to 320 ℃, and the carbonization temperature is 800 ℃ to 1200 ℃. By adopting the densification process and the parameters, the carbonized solidified piece can be densified with lower process cost and higher densification efficiency, so that a product meeting the density of a target product carbon/carbon composite material is obtained.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the net tire is laid in the fiber layer with the adhesive, and the carbon fiber is introduced in the radial direction by combining the needling treatment process, so that the forming-compact integration of the winding process is realized, the interlayer bonding strength of the wound formed carbon/carbon composite material is obviously improved, the interlayer bonding strength of the finally obtained wound formed carbon/carbon composite material is not lower than 10MPa, and the obvious defects of layering, bulging and yarn falling are avoided.
2. The invention winds the adhesive fiber layer on the core mould and lays the net tyre to carry out the needle punching treatment, and then the needle punching treatment is carried out in sequenceSolidifying and carbonizing to obtain the product with a density of 1.00g/cm3～1.40g/cm3And the carbonized part with the interlayer bonding strength not less than 8MPa in a quasi-three-dimensional structure is subjected to high-temperature purification and mechanical processing to obtain the wound and formed carbon/carbon composite material, the carbonized part does not have the obvious defects of no layering, no bulging and no yarn falling in the subsequent purification and processing processes, the interlayer bonding strength of the wound and formed carbon/carbon composite material is further ensured, the process is simple, and the realization is easy.
3. The invention adopts the annular and spiral alternate winding, and the winding line type design of the continuous carbon fiber pre-impregnated with resin is beneficial to realizing the arrangement of the continuous carbon fiber pre-impregnated with resin on the surface of the core mould in a tight and non-overlapping way, and simultaneously plays the role of radial and axial reinforcement.
4. When the winding-formed carbon/carbon composite material is applied as a carbon/carbon crucible side for monocrystalline silicon, the erosion resistance and deformation resistance of an application product are obviously improved, and the service life of the application product is prolonged.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a block diagram of a process for preparing the present invention.
Fig. 2 is a schematic view showing a structure of spirally winding on the surface of the core mold according to the present invention.
Fig. 3 is a schematic view of the structure of the core mold used in example 1 of the present invention.
Fig. 4 is a schematic structural view of a winding-needling member prepared in example 1 of the present invention.
FIG. 5 is a schematic view of the structure of the wrapped shaped carbon/carbon composite crucible prepared in example 1 of the present invention.
Description of the reference numerals
1, a mandrel; 2-straight cylinder section; 3, processing a reserved seam;
4-a head sealing section; 5, fastening pieces.
Detailed Description
As shown in fig. 1, the preparation process of the invention is as follows: selecting a core mould, sequentially cleaning, laying release cloth, brushing a release agent and laying a soft temperature-resistant material, winding continuous carbon fibers which are pre-impregnated with resin on the prepared core mould, laying a net tire, carrying out needling treatment, and sequentially carrying out curing, carbonization, high-temperature process treatment and machining to obtain the winding molding carbon/carbon composite material.
As shown in fig. 2, the present invention adopts a spiral winding method to realize the cross winding of the continuous carbon fiber pre-impregnated with resin on the surface of the core mold.
Example 1
The embodiment comprises the following steps:
step one, core mould preparation: determining the design density of the target product carbon/carbon composite material crucible to be 1.40g/cm3Selecting No. 45 steel to process and manufacture a core mould and assemble the core mould, cleaning the outer surface of the assembled core mould, laying demolding cloth on the outer surface of the cleaned core mould, brushing a demolding agent on the core mould, and laying graphite paper coated with phenolic resin until the laying thickness is 5mm, wherein the wall thickness is 18mm, the height is 400mm, the inner diameter of the straight cylinder section is 660mm, and the index of the annular tensile strength is not less than 100 MPa; the shape of the core mold is similar to the shape of two target product carbon/carbon composite material crucibles spliced oppositely, the outer diameter of a straight cylinder section of the core mold is 650mm, the length of the core mold is more than twice the height of the target product carbon/carbon composite material crucible, the length of the core mold comprises machining allowance, the shape of a sealing head section of the core mold is the same as the shape of an arc surface section of the target product carbon/carbon composite material crucible, the size of the arc surface section is reduced in the same proportion, the specific structure of the core mold is shown in figure 3, the core mold adopted in the embodiment comprises a core shaft 1 and a straight cylinder section 2 installed on the core shaft 1, a machining reserved seam 3 is arranged in the center of the straight cylinder section 2, sealing head sections 4 are arranged at two ends of the straight cylinder section 2, and the straight cylinder section 2 and the sealing head sections 4 are fixed on the core shaft 1 through fasteners 5 arranged at the end parts of the two sealing head sections 4;
step two, continuously winding the tape adhesive and performing needle punching forming: adopting a winding machine to wind 12K pitch-based carbon fibers pre-impregnated with the furfuryl ketone resin ethanol solution on the outer surface of the core mold for laying the graphite paper in the step I in a dry method, and adopting a spiral and annular alternate winding mode, wherein the annular winding angle is 87 degrees, the spiral winding angle is 55 degrees, and the pitch-based carbon fibers are formedA carbon fiber layer, wherein a net tire is laid on the pitch-based carbon fiber layer formed by winding after every 2 layers are wound in the winding process, the net tire and the pitch-based carbon fiber layer on the lower layer of the net tire are subjected to needling treatment by using a needle machine, furfuryl ketone resin is coated on the net tire subjected to the needling treatment, then single-layer hoop winding is carried out on a straight cylinder section area of a core mold, and the spiral winding, the net tire laying, the needling treatment, the coating and the hoop winding processes are repeated until a winding-needling piece with a quasi-three-dimensional structure and the thickness of 18mm is formed, as shown in fig. 4; the net tire is a thin felt made of chopped carbon fibers, and the surface density of the net tire is 20g/m2In the process of laying the net tires, the net tires with the same width as the length of the core mold and the same length as the wound core mold perimeter before laying the net tires are uniformly laid on the straight cylinder section of the core mold, the net tires which are cut to be fan-shaped and have the same area as the head sealing section are laid on the head sealing section of the core mold, the distance between the adjacent net tires on the same layer is not more than 0.2mm, and the gaps for laying the net tires on the adjacent layers are staggered; the needling depth of the needling treatment is 1mm, the needling frequency is 1 layer/time, and the needling density is 50 needles/cm2；
Step three, curing treatment: placing the winding-needling piece formed on the core mold in the second step on a tool frame in a curing furnace, rotating the core mold at the speed of 1 r/min by driving of an electrode for rotary curing treatment, then cooling to room temperature, loading the core mold into a machine for demolding by adopting a demolding tool, and removing graphite paper to obtain a cured piece with a quasi-three-dimensional structure; the density of the quasi-three-dimensional structure solidified piece is 1.30g/cm3；
Step four, carbonizing treatment: placing the quasi-three-dimensional structure solidified piece obtained in the third step in a carbonization furnace, carbonizing under the protection of nitrogen, cooling to room temperature, placing the solidified piece which is carbonized and cooled to room temperature in an impregnation tank, impregnating for 4 hours by using furfuryl ketone resin under the condition that the pressure is 1.0MPa, then solidifying at 320 ℃, then placing in the carbonization furnace, carbonizing at 800 ℃ to complete single densification, and repeating the single densification process of impregnation, solidification and carbonization to obtain the quasi-three-dimensional structure carbonized piece; the system of the carbonization treatment is as follows: (1) firstly, heating to 300 ℃ at the speed of 20-40 ℃/min and preserving heat for 2 h; (2) however, the device is not suitable for use in a kitchenThen heating to 550 ℃ at the speed of 5-15 ℃/min and preserving heat for 2 h; (3) then heating to 850 ℃ at the speed of 5-10 ℃/min and preserving the heat for 2 h; the density of the solidified part after carbonization treatment and cooling to room temperature is 1.00g/cm3The interlayer bonding strength is 8MPa, and obvious defects of layering, bulging and yarn falling are avoided; the density increase of the single densification is less than 0.3g/cm3When in use, the solidified piece after single densification is subjected to tapping treatment at 1800-2500 ℃, then the single densification process is repeated, and the density of the carbonized piece with the quasi-three-dimensional structure is 1.45g/cm3；
Step five, high-temperature treatment: carrying out high-temperature purification treatment on the carbonized part with the quasi-three-dimensional structure obtained in the fifth step at the temperature of 2000 ℃;
step six, machining: and (3) performing machining treatment on the carbonized part subjected to high-temperature purification treatment in the sixth step along the machining reserved seam to obtain 2 wound and molded carbon/carbon composite material crucibles with the same specification, as shown in fig. 5.
Through detection, the interlaminar density of the winding-molded carbon/carbon composite material crucible obtained in the embodiment is 1.45g/cm3The interlayer bonding strength is 20MPa, the hoop tensile strength is 120MPa, and obvious defects of layering, bulging and yarn falling are avoided.
The soft temperature-resistant material in the first step of this embodiment may also be one or more than two of carbon felt, carbon cloth, carbon fiber net blank, graphite paper, and ceramic fiber felt other than graphite paper.
The material of the continuous carbon fiber pre-impregnated with resin in the second step of this embodiment may also be one or more than two of viscose fiber, polyacrylonitrile fiber and pitch fiber, except pitch fiber.
Example 2
The present embodiment differs from embodiment 1 in that: the designed density of the target product carbon/carbon crucible edge in the step one is 1.65g/cm3The interlayer bonding strength is not less than 20MPa, the circumferential tensile strength index is not less than 150MPa, the core mold is made of electrode graphite, the outer diameter of the core mold is 600mm, and a carbon felt impregnated with the furfuryl ketone resin is laid until the laying thickness is 30 mm; step (ii) ofAnd secondly, performing semi-dry winding on 24K polyacrylonitrile-based carbon fibers impregnated with furfuryl ketone resin ethanol solution, wherein the winding mode is that the hoop winding angle and the spiral winding angle are alternately wound, the hoop winding angle is 89 degrees, the spiral winding angle is 85 degrees, a net tire is laid after every 5 layers of winding, and the density of the net tire surface is 300g/cm3Then, needling treatment is carried out by a needling machine under the core mold rotating state, the needling depth is 10mm, the needling frequency is 5 layers/time, and the needling density is 5 needles/cm2Spraying asphalt powder on the net tire after the needling treatment, and repeating the steps until a winding-needling piece with a quasi-three-dimensional structure with the thickness of 30mm is obtained; the rotation rate of the core mold in the curing process in the third step is 30 revolutions per minute; in the fourth step, the dipping pressure is 3.0MPa, the curing temperature is 240 ℃, and the carbonization temperature is 1000 ℃; the density of the solidified part after carbonization treatment is 1.20g/cm3The interlayer bonding strength was 14 MPa.
The density of the winding molding carbon/carbon hot-pressing mold obtained in the embodiment is 1.67g/cm through detection3The interlayer bonding strength is 25MPa, and the hoop tensile strength is 160 MPa.
Example 3
The present embodiment differs from embodiment 1 in that: the designed density of the target product carbon/carbon crucible edge in the step one is 1.35g/cm3The interlayer bonding strength is not less than 12MPa, the circumferential tensile strength index is not less than 60MPa, the core mold is made of electrode graphite, the outer diameter of the core mold is 630mm, the soft temperature-resistant material laid on the core mold is a carbon fiber net tire, and the laying thickness is 15 mm; and step two, adopting 1.5K viscose-based carbon fiber to perform circumferential and spiral alternate winding, wherein the circumferential winding angle is 85 degrees, the spiral winding angle is 20 degrees, the viscose-based carbon fiber is fully soaked in a phenolic resin ethanol solution for wet winding before winding, laying a net tire and spraying resin powder after each 8-time circumferential and spiral alternate winding, and the net tire surface density is 160g/cm3Then, needling treatment is carried out by a needling machine under the core mold rotating state, the needling depth is 5mm, the needling frequency is 3 layers/time, and the needling density is 25 needles/cm2Spraying phenolic resin powder on the needled net tire, and repeating the spraying and needling steps until the thickness of the net tire reaches 22mm, wherein the net tire is of a quasi-three-dimensional structure; step (ii) ofIn the third step, the core mold rotation speed in the curing process is 60 revolutions per minute; in the fourth step, the dipping pressure is 2.0MPa, the curing temperature is 160 ℃, and the carbonization temperature is 1200 ℃; the density of the solidified part after carbonization treatment is 1.05g/cm3The interlayer bonding strength was 8 MPa.
Through detection, the density of the winding-formed carbon/carbon crucible edge obtained in the embodiment is 1.37g/cm3The interlayer bonding strength is 14MPa, and the hoop tensile strength is 70 MPa.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (10)
1. A method for improving interlayer bonding strength of a winding-formed carbon/carbon composite material is characterized by comprising the following steps:
step one, core mould preparation: selecting a core mould with the outer surface structure and the size similar to those of the inner surface structure and the size of the target product carbon/carbon composite material, assembling, cleaning the outer surface of the assembled core mould, laying demolding cloth on the outer surface of the cleaned core mould, brushing a demolding agent on the outer surface of the core mould, and laying a soft temperature-resistant material; the outer diameter of the core mold is 10 mm-60 mm smaller than the inner diameter of the target product carbon/carbon composite material;
step two, continuously winding the tape adhesive and performing needle punching forming: winding continuous carbon fibers pre-impregnated with resin on the outer surface of the core mold laid with the soft temperature-resistant material in the first step by using a winding machine to form a fiber layer with glue, laying a net tire on the fiber layer with glue formed by winding after winding a single layer or multiple layers in the winding process, and carrying out needling treatment on the net tire and the fiber layer with glue at the lower layer of the net tire to form a winding-needling piece with a quasi-three-way structure on the core mold; the thickness of the winding-needling piece of the quasi-three-way structure is not less than that of the target product carbon/carbon composite material; in the process of laying the net tires, the net tires with the same width as the length of the core mold and the same length as the wound core mold circumference before laying the net tires are uniformly laid on the straight cylinder section of the core mold, the net tires which are cut to be fan-shaped and have the same area as the head sealing section are laid on the head sealing section of the core mold, the distance between the adjacent net tires in the same layer is not more than 0.2mm, and the gaps for laying the net tires in the adjacent layers are staggered;
step three, curing treatment: placing the winding-needling piece formed on the core mold in the second step into a curing furnace for curing treatment, then demolding and removing the soft temperature-resistant material to obtain a cured piece with a quasi-three-dimensional structure; the density of the quasi-three-dimensional structure solidified piece is 1.30g/cm3～1.50g/cm3；
Step four, carbonizing treatment: placing the quasi-three-dimensional structure solidified piece obtained in the third step in a carbonization furnace, and carrying out carbonization treatment under the protection of nitrogen or argon atmosphere and at the temperature of 850-1200 ℃ to obtain a quasi-three-dimensional structure carbonized piece; the density of the carbonized part with the quasi-three-dimensional structure is 1.00g/cm3～1.40g/cm3The interlayer bonding strength is not less than 8MPa, and obvious defects of layering, bulging and yarn falling are avoided;
step five, high-temperature treatment: carrying out high-temperature purification treatment on the carbonized part with the quasi-three-dimensional structure obtained in the fifth step at the temperature of 2000-2500 ℃;
step six, machining: machining the carbonized part subjected to high-temperature purification treatment in the sixth step to obtain a winding formed carbon/carbon composite material; the interlayer bonding strength of the winding forming carbon/carbon composite material is not less than 10MPa, and obvious defects of layering, bulging and yarn falling are avoided.
2. The method for improving the interlayer bonding strength of the wound carbon/carbon composite material as claimed in claim 1, wherein the core mold in the first step is made of metal or graphite.
3. The method for improving the interlayer bonding strength of the wound carbon/carbon composite material according to claim 1, wherein in the step one, the soft temperature-resistant material is one or more than two of carbon felt, carbon cloth, carbon fiber net tire, graphite paper and ceramic fiber felt, and the laying thickness of the soft temperature-resistant material is 5mm to 30 mm.
4. The method for improving the interlayer bonding strength of the winding-formed carbon/carbon composite material according to claim 1, wherein the soft temperature-resistant material is coated after being impregnated with the resin in the first step, or the soft temperature-resistant material is coated or impregnated with the resin after being coated, wherein the resin is phenolic resin or furfuryl ketone resin, and the curing temperature of the resin is not higher than that of the resin used for the continuous carbon fiber in which the resin is impregnated in advance in the second step.
5. The method for improving interlayer bonding strength of the winding-formed carbon/carbon composite material as claimed in claim 1, wherein in the second step, the material of the continuous carbon fiber pre-impregnated with the resin is one or more of viscose filament-based carbon fiber, polyacrylonitrile-based carbon fiber and pitch-based carbon fiber, the tow of the continuous carbon fiber pre-impregnated with the resin is 1.5K-24K, the net body is a thin felt made of chopped carbon fiber, and the surface density of the net body is 20g/m2～300g/m2。
6. The method for improving the interlayer bonding strength of the wound and formed carbon/carbon composite material according to claim 1, wherein the winding in the second step is dry winding, semi-dry winding or wet winding; the resin glue solution adopted by the continuous carbon fiber pre-impregnated with the resin is a thermosetting resin glue solution with a carbon residue rate of not less than 45%, and the thermosetting resin glue solution is an ethanol solution of furfuryl ketone resin or phenolic resin; the winding mode is that the hoop and the spiral are alternately wound, wherein the hoop winding angle is 85-89 degrees, and the spiral winding angle is 20-85 degrees.
7. The method for improving the interlayer bonding strength of the wound and formed carbon/carbon composite material as claimed in claim 1, wherein the needling treatment in the second step has a needling depth of 1mm to 10mm, a needling frequency of 1 layer/time to 5 layers/time, and a needling density of 5 needles/cm2About 50 needles/cm2。
8. The method for improving the interlayer bonding strength of the wound and formed carbon/carbon composite material as claimed in claim 1, wherein the resin is applied by brush coating, resin powder or asphalt powder is sprayed on the net tire after the needle punching treatment in the second step, and the resin powder are the same as the resin in the resin solution adopted by the continuous carbon fiber which is previously impregnated with the resin.
9. The method for improving the interlayer bonding strength of the wound carbon/carbon composite material as claimed in claim 1, wherein the curing treatment in the third step is a rotational curing treatment, and the rotational curing treatment adopts a rotational speed of 1 to 60 revolutions per minute.
10. The method for improving the interlayer bonding strength of the wound carbon/carbon composite material as claimed in claim 1, wherein when the density of the cured piece subjected to the carbonization treatment in the fourth step is less than that of the target product carbon/carbon composite material, the cured piece subjected to the carbonization treatment is subjected to densification treatment, and the specific process is as follows: impregnating and curing the carbonized curing piece by using furfuryl ketone resin or pitch, then carbonizing to finish single densification, and repeating the single densification process of impregnation, curing and carbonization until the density of the densified curing piece is 1.00g/cm3～1.40g/cm3The solidified part after densification treatment is a carbonized part with a quasi-three-dimensional structure; when the density increase of the single densification is less than 0.3g/cm3When in use, the solidified piece after single densification is subjected to tapping treatment at 1800-2500 ℃, and then the single densification process is repeated; the infiltration pressure is 1.0MPa to 3.0MPa, the curing temperature is 160 ℃ to 320 ℃, and the carbonization temperature is 800 ℃ to 1200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911422008.6A CN111169031B (en) | 2019-12-31 | 2019-12-31 | Method for improving interlayer bonding strength of winding-formed carbon/carbon composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911422008.6A CN111169031B (en) | 2019-12-31 | 2019-12-31 | Method for improving interlayer bonding strength of winding-formed carbon/carbon composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111169031A CN111169031A (en) | 2020-05-19 |
| CN111169031B true CN111169031B (en) | 2022-03-04 |
Family
ID=70652452
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911422008.6A Active CN111169031B (en) | 2019-12-31 | 2019-12-31 | Method for improving interlayer bonding strength of winding-formed carbon/carbon composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111169031B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225574B (en) * | 2020-09-28 | 2022-06-03 | 烟台凯泊复合材料科技有限公司 | Manufacturing method of high-performance carbon/carbon combined hot-pressing mold |
| CN112225575B (en) * | 2020-09-28 | 2022-06-03 | 烟台凯泊复合材料科技有限公司 | High-performance carbon/carbon combined hot pressing die |
| CN114591095B (en) * | 2020-12-03 | 2023-05-23 | 航天特种材料及工艺技术研究所 | Method for improving fiber volume content in large-thickness 2D fiber reinforced ceramic matrix composite |
| CN113149682A (en) * | 2021-04-29 | 2021-07-23 | 上海骐杰碳素材料有限公司 | Carbon or carbon ceramic composite material winding preform, product and preparation method thereof |
| CN113149684A (en) * | 2021-04-29 | 2021-07-23 | 上海骐杰碳素材料有限公司 | Carbon-carbon or carbon-ceramic composite material winding preform, product and preparation method thereof |
| CN113681932A (en) * | 2021-08-16 | 2021-11-23 | 西安联瑞科技实业有限责任公司 | Preparation method of composite material plate spring body based on winding forming and plate spring body |
| CN113681931A (en) * | 2021-08-16 | 2021-11-23 | 西安联瑞科技实业有限责任公司 | Preparation method of composite material plate spring body based on prepreg molding |
| CN113800925B (en) * | 2021-09-14 | 2022-08-09 | 艾文斯（焦作）冶金材料有限责任公司 | Casing pipe forming process |
| CN113999034B (en) * | 2021-11-12 | 2023-03-10 | 青海中昱新材料科技有限公司 | Preparation method of long-life carbon crucible side |
| CN114274557B (en) * | 2021-12-24 | 2023-05-30 | 哈尔滨工程大学 | Connection design and molding method of composite material cylindrical shell and metal component |
| CN115449968B (en) * | 2022-09-15 | 2023-11-07 | 南京航空航天大学 | Knitting and needling integrated preform forming method and preform forming device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060555A (en) * | 2010-11-24 | 2011-05-18 | 西安超码科技有限公司 | Method for manufacturing high-strength carbon/carbon hot-press die |
| CN102173846A (en) * | 2010-12-30 | 2011-09-07 | 西安航天复合材料研究所 | Preparation method of C/C composite tube of optical telescope |
-
2019
- 2019-12-31 CN CN201911422008.6A patent/CN111169031B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060555A (en) * | 2010-11-24 | 2011-05-18 | 西安超码科技有限公司 | Method for manufacturing high-strength carbon/carbon hot-press die |
| CN102173846A (en) * | 2010-12-30 | 2011-09-07 | 西安航天复合材料研究所 | Preparation method of C/C composite tube of optical telescope |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111169031A (en) | 2020-05-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111169031B (en) | Method for improving interlayer bonding strength of winding-formed carbon/carbon composite material | |
| US6824862B2 (en) | Fiber-reinforced ceramic composite | |
| JPH01167276A (en) | Hollow composite body having symmetrical center of axis | |
| CN108191448A (en) | A kind of method that winding process prepares carbon/carbon cylinder | |
| JPH0253386B2 (en) | ||
| CN109056186B (en) | Preparation method of low-density multi-angle woven carbon fiber hard heat-insulation cylinder | |
| JPH03140609A (en) | Carbon/carbon complex fastener | |
| CN111170756B (en) | Preparation method of revolving body carbon/carbon composite material | |
| CN104261853B (en) | Asphalt base carbon fiber non-woven mat heat-preservation cylinder and manufacture method thereof | |
| CN108610080B (en) | Preparation method of carbon-carbon composite material with inner hole and carbon-ceramic composite material | |
| CN110105079A (en) | A kind of preparation method of Carbon fibe sewing hardening heat preservation cylinder | |
| EP2993016B1 (en) | Sacrificial fibers to create channels in a composite material | |
| CN113149685A (en) | Carbon-carbon or carbon-ceramic composite material net tire preform, product and preparation method thereof | |
| CN108129158B (en) | Carbon-carbon thin-wall porous piece and preparation method thereof | |
| US20060068150A1 (en) | Tribological fiber composite component produced according to the tfp process | |
| CA2726177C (en) | Process for producing a ceramic matrix composite article and article formed thereby | |
| CN111875401B (en) | Preparation method of high-strength and high-purity carbon/carbon composite material revolving body formed by winding | |
| CN112522857A (en) | Preparation method of high-thickness hard felt | |
| CN113862773A (en) | Long-life guide cylinder and preparation method thereof | |
| CN204224476U (en) | Asphalt base carbon fiber non-woven mat heat-preservation cylinder | |
| CN113149684A (en) | Carbon-carbon or carbon-ceramic composite material winding preform, product and preparation method thereof | |
| EP4137313A1 (en) | Method for manufacturing composite fiber preform for disc brakes | |
| CN114436670A (en) | Winding forming-based high-strength carbon-carbon cylinder preparation method | |
| CN114853495A (en) | Preparation method of carbon/carbon hot pressing mold for high-pressure hot pressing sintering furnace | |
| CN113149682A (en) | Carbon or carbon ceramic composite material winding preform, product and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |