CN111170756A - Preparation method of revolving body carbon/carbon composite material - Google Patents
Preparation method of revolving body carbon/carbon composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a revolving body carbon/carbon composite material, which comprises the following steps: firstly, paving demolding cloth and brushing a demolding agent on a core mold after cleaning; secondly, winding the continuous carbon fiber on a core mold coated with a release agent to form a winding piece; thirdly, carrying out vacuum pressure impregnation on the wound part, and carrying out machining treatment after demolding to obtain an impregnated part; fourthly, applying a shaping tool to the outer surface of the impregnated part and performing internal pressurization heat treatment to obtain a rotator carbon/carbon composite material blank; and fifthly, strengthening the rotator carbon/carbon composite material blank to obtain the rotator carbon/carbon composite material. The invention achieves the thickness of the target product by introducing the asphalt and adopting the internal pressurization heat treatment process of external shaping and strengthening treatment, increases the volume content of carbon fibers in the revolving body type carbon/carbon composite material, improves the performance of the revolving body carbon/carbon composite material, shortens the densification period and improves the preparation efficiency of the revolving body carbon/carbon composite material.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of a revolving body carbon/carbon composite material.
Background
The carbon/carbon composite material is a composite material of a carbon fiber reinforced carbon matrix, has a series of excellent performances of high strength and high modulus, light specific gravity, small thermal expansion coefficient, corrosion resistance, thermal shock resistance, good friction resistance, good chemical stability and the like, and is a novel ultrahigh-temperature composite material. The rotary carbon/carbon composite material is widely applied to the civil fields of monocrystalline silicon pulling, advanced ceramic hot pressing and the like in the forms of products such as a carbon/carbon crucible, a carbon/carbon hot pressing mold and the like.
Although carbon/carbon composites have many excellent properties, they are mainly used in the civil field in severe working environments where other materials are difficult to replace, due to their high price. The characteristics of long manufacturing period and high cost of the carbon/carbon composite material greatly limit the wide application of the excellent material in various fields of national economy. In recent decades, shortening the manufacturing period, reducing the cost and expanding the application range while taking structural properties into consideration have become the main research focus in the field of carbon/carbon composite materials.
The winding/winding forming process is to wind/wind the continuous fiber (or cloth belt, presoaked yarn) soaked with resin glue solution onto the core mold according to a certain rule, and then to obtain the product after curing and demolding. The carbon/carbon composite material obtained by the winding/winding forming process has the characteristics of high specific strength, good structure designability, high production efficiency and product reliability and low raw material cost. The patent with the application number of 200610104824.9 discloses a preparation method of a C/C composite material conductive threaded rod, which adopts a prefabricated body of 'axial carbon fiber rod + carbon fiber winding/winding circumferential threads' to increase the density of the threaded rod through chemical vapor deposition, liquid phase impregnation/carbonization and the likeAnd finally obtaining the high-density C/C composite material conductive threaded rod. The patent application No. 201280038583.6 discloses a method for improving interlayer bonding strength of winding/winding composite material, which is to inlay the interlayer fibers by changing the winding/winding angles of different layers, thereby improving the interlayer bonding strength. The patent application No. 201310336558.2 discloses a method for manufacturing a carbon/carbon crucible by winding/coiling carbon fiber on the surface of a core mold layer by layer to obtain a crucible preform, and then curing and densifying the crucible to obtain a carbon/carbon crucible with a density of 1.70g/cm or more3The carbon/carbon crucible finished product. The patent with the application number of 201510103863.6 relates to a preparation method of a high-strength light carbon/carbon composite material, which is obtained by pretreating fibers, mixing and modifying resin, applying a winding/winding forming process to obtain the high-strength light carbon/carbon composite material with the tensile strength of more than 800MPa, the thermal conductivity of 500W/(m.K) -530W/(m.K), and the thermal diffusivity of 4.4cm2And s. It can be seen from the above patents that excellent mechanical properties can be obtained by winding/coiling the formed carbon/carbon composite material. Meanwhile, the preparation period is shortened while the performance is ensured, and the high-efficiency preparation is realized, and at present, no complete related research of the preparation method exists.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a revolving body type carbon/carbon composite material aiming at the defects of the prior art. The method prepares the winding body with the thickness larger than that of the target product revolution body type carbon/carbon composite material, and then introduces asphalt and adopts an external shaping internal pressurization heat treatment process and strengthening treatment to reach the thickness of the target product, thereby increasing the volume content of carbon fibers in the revolution body type carbon/carbon composite material, improving the performance of the revolution body type carbon/carbon composite material, shortening the densification period in the subsequent process and further improving the preparation efficiency of the revolution body type carbon/carbon composite material.
In order to solve the technical problems, the invention adopts the technical scheme that: the preparation method of the revolving body carbon/carbon composite material is characterized by comprising the following steps:
step one, core mould preparation: cleaning the outer surface of the core mold by using a cleaning agent, then laying release cloth on the outer surface of the cleaned core mold, and brushing a release agent on the release cloth;
step two, winding carbon fibers: winding the continuous carbon fiber on the core mold coated with the release agent in the step one by using a winding machine, and forming a winding piece on the core mold; the thickness of the winding piece is larger than that of the target product revolution body type carbon/carbon composite material;
step three, vacuum pressure impregnation: embedding the winding piece obtained in the step two and the core mold into asphalt, then placing the winding piece and the core mold into a vacuum pressure impregnation furnace for vacuum pressure impregnation, and performing internal and external surface machining treatment after demolding to obtain an impregnated piece;
step four, internal pressurization heat treatment: applying a shaping tool to the outer surface of the impregnated part obtained in the third step, putting or introducing a pressure transmission medium material into the impregnated part, and then carrying out internal pressurization heat treatment on the impregnated part and the shaping tool through the pressure transmission medium material to simultaneously increase the inner diameter and the outer diameter of the impregnated part and ensure that the increase value of the outer diameter is smaller than the increase value of the inner diameter, so that the thickness of the impregnated part is reduced, and a revolved body carbon/carbon composite material blank is obtained; the internal pressure heat treatment process comprises the following steps: pressurizing the dipping part internally, carrying out heat treatment on the dipping part and the shaping tool, increasing the pressure and maintaining the pressure when the temperature of the heat treatment is raised to the asphalt softening temperature in the dipping part, and then raising the temperature in a pressure maintaining state to sequentially carry out carbonization and graphitization; the thickness of the revolution body carbon/carbon composite material blank is not less than that of the revolution body carbon/carbon composite material of the target product;
step five, strengthening treatment: strengthening the rotator type carbon/carbon composite material blank obtained in the fourth step to obtain a rotator type carbon/carbon composite material; the strengthening method is densification treatment or/and coating preparation treatment, wherein the densification treatment adopts resin liquid-phase impregnation carbonization or chemical vapor infiltration, and the coating preparation treatment adopts chemical vapor deposition or brush coating.
The invention adopts a method of winding and molding on a core mold to prepare a winding piece of carbon/carbon composite material with the thickness larger than that of a target product revolution body, which is beneficial to avoiding fiber loss and improving the fiber strength exertion rate, then vacuum pressure impregnation is carried out to introduce asphalt to obtain an impregnation piece, a shaping tool is applied to the outer surface of the impregnation piece to limit deformation, internal pressurization heat treatment of external shaping is carried out, under the premise that the inner diameter and the outer diameter of the impregnation piece are simultaneously increased, the outer diameter increase value of the impregnation piece is smaller than the inner diameter increase value, so that a revolution body type carbon/carbon composite material blank with the thickness reduced but not smaller than the thickness of a final product is obtained, in the internal pressurization heat treatment process, when the asphalt is heated to be softened and become a low-viscosity state, internal pressurization is carried out, and the asphalt and the carbon fiber flow/slip and rearrangement in the circumferential direction are, because the outer diameter of the impregnated part is limited by the shaping tool and can not be freely changed, the thickness of the impregnated part is reduced, the fiber is impregnated more sufficiently and uniformly by the asphalt, the fiber is fully stretched and is in a tensile stress state, and the strength exertion rate of the fiber is further improved; along with the compression of the impregnated part, the volume content of the carbon fiber is increased, the content of the asphalt is reduced, and the reduction of the volume content of the asphalt is beneficial to the reduction of the number of defects in the subsequent heat treatment process because the defects are generated in the heat treatment process of the asphalt, thereby improving the bonding performance between fiber layers; when internal pressurization is carried out in the carbonization and graphitization processes, asphalt is enabled to generate corresponding structural transformation in a pressurized state, the improvement of the carbon residue rate in a blank of the revolving body type carbon/carbon composite material is facilitated, the density of a carbonized piece and/or a graphite piece obtained through internal pressurization heat treatment is higher, and the subsequent densification period is avoided or shortened.
The preparation method of the revolving body type carbon/carbon composite material is characterized in that the shape of the outer surface of the core mold in the step one is the same as or similar to the shape of the inner surface of the target product revolving body type carbon/carbon composite material. In the core mold preparation process, the core mold is designed and prepared according to the structural design of the target product revolution body type carbon/carbon composite material and the deformation rule of the fiber material in the subsequent internal pressurization heat treatment process, so that the shape of the inner surface of the core mold is preferably the same as or similar to the shape of the outer surface of the target product revolution body type carbon/carbon composite material, the rapid forming and demolding of the target product are facilitated, and the preparation efficiency is improved.
The preparation method of the revolving body type carbon/carbon composite material is characterized in that in the step two, the continuous carbon fiber is one or more than two of PAN (polyacrylonitrile) -based carbon fiber, pitch-based carbon fiber and viscose-based carbon fiber. The preparation of the revolving body carbon/carbon composite material with different purposes is satisfied by adopting the preferable material, the revolving body carbon/carbon composite material comprises a structural part and a functional part, and the combination of different carbon fibers is used, so that the application range of the revolving body carbon/carbon composite material is favorably expanded.
The preparation method of the revolution body type carbon/carbon composite material is characterized in that in the step two, the winding mode is spiral winding or annular spiral alternate winding, wherein the annular winding angle is 85-89 degrees, the spiral winding angle is 20-85 degrees, in the annular spiral alternate winding process, the control host of the winding machine automatically controls the machine head of the winding machine, and the winding direction of continuous carbon fibers is gradually and automatically converted into the annular winding direction from the spiral winding direction or gradually and automatically converted into the spiral winding direction from the annular winding direction under the condition of not cutting off the continuous carbon fibers, so that the continuous transition between the spiral winding layer and the annular winding layer is realized. The carbon/carbon composite material prepared by adopting the optimized winding method, the optimized winding angle and the winding operation key points meets different requirements on a preparation device, preparation efficiency and process cost, and is beneficial to obtaining carbon/carbon composite materials with different structural performance designs.
The preparation method of the revolving body type carbon/carbon composite material is characterized in that the thickness of the winding piece in the step two is 1.05-1.75 times that of the revolving body type carbon/carbon composite material obtained in the step five. The preferable thickness multiple is beneficial to the winding piece to obtain the revolving body carbon/carbon composite material with high fiber strength utilization rate and short preparation period through an internal pressurization heat treatment process.
The preparation method of the revolved body type carbon/carbon composite material is characterized in that the average value Vf of the fiber volume content in the revolved body type carbon/carbon composite material blank in the fourth step is more than 65% or the layer number distribution is not less than 50 layers/cm. The rotator type carbon/carbon composite material blank obtained by the internal pressurization heat treatment process has the advantages of fully extended fibers, uniform bearing capacity, high strength exertion rate, uniform and compact resin pyrolytic carbon among fiber winding layers, less defects and good interlayer bonding performance of the blank material.
The preparation method of the revolved body carbon/carbon composite material is characterized in that the inner diameter of the shaping tool in the fourth step is larger than the outer diameter of the impregnated part, and the size of a gap between the shaping tool and the impregnated part is 0.5-5 mm. The inner diameter of the shaping tool is larger than the outer diameter of the dipping piece, so that the shaping effect of the shaping tool is ensured; the preferred gap size accommodates high temperature expansion deformation of the impregnated article during internal pressure heat treatment while achieving good sizing.
The preparation method of the revolving body carbon/carbon composite material is characterized in that the pressure transmission medium material adopted for carbonization and graphitization in the step four is a solid phase, and the pressure transmission medium material of the solid phase is graphite powder or carbonized silicon powder. The optimal pressure-transmitting medium material can bear carbonization and graphitization temperatures, does not react with the impregnation piece, is beneficial to uniformly applying pressure to the inner molded surface of the impregnation piece in the internal pressure heat treatment process, and avoids the defect caused by insufficient or excessive local pressure.
The preparation method of the revolving body carbon/carbon composite material is characterized in that the internal pressurization heat treatment in the step four is carried out under the protection of vacuum or inert atmosphere, and the carbonization and the graphitization both adopt a step type heating heat treatment process. A carbonization system is established according to the viscosity-temperature curve and the pyrolysis curve of the asphalt, a graphitization system is established according to the structural transformation rule of a carbonized piece obtained after carbonization, and the reduction of the strength of a blank body caused by the oxidation reaction of the impregnated piece and air in the heat treatment process is favorably inhibited through vacuum or inert atmosphere protection; the stepped heating heat treatment process is favorable for inhibiting the stress concentration of the dipping piece in the process, so that the revolving body carbon/carbon composite material with better performance is obtained.
The preparation method of the revolving body carbon/carbon composite material is characterized in that the internal pressurization heat treatment system in the step four is as follows: (1) firstly, heating to the asphalt softening temperature at the speed of 20-35 ℃/min under the pressure of 4-8 MPa; (2) then heating to the temperature of the lowest viscosity value of the asphalt at the speed of 10-35 ℃/min under the pressure of 4-8 MPa, and preserving the heat for 1-3 h; (3) continuously heating to 400 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and keeping the temperature for 0.5-2 h; (4) continuously heating to 550 ℃ at the speed of 1-3 ℃/min under the pressure of 4-8 MPa, and keeping the temperature for 0.5-2 h; (5) continuously heating to 900 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and preserving the temperature for 1-2 h to finish carbonization; (6) heating to 2600 deg.C at the speed of 5-50 deg.C/min under the pressure of 2-5 MPa, maintaining for 1-2 h to complete graphitization, and cooling to room temperature along with the furnace. Through the optimized internal pressurization heat treatment system, the circulation/sliding and rearrangement of the asphalt and the fibers in the impregnated part in the circumferential direction under the action of the radial pressure of the inner molded surface are facilitated, the fiber volume of the blank body is higher, the asphalt is fully impregnated into the fibers and is distributed more uniformly, the fibers are fully stretched and are in a tensile stress state, and the fiber strength exertion rate and the performance of the winding-molded carbon/carbon composite material are further improved.
The preparation method of the revolving body type carbon/carbon composite material is characterized in that the specific process of chemical vapor infiltration strengthening in the step five is as follows: vacuumizing the chemical vapor infiltration furnace, heating to 950-1300 ℃ at the speed of 100-300 ℃/h, keeping the vacuum degree in the chemical vapor infiltration furnace lower than 2000Pa, and introducing inert gas and hydrocarbon gas into the chemical vapor infiltration furnace according to the volume ratio of 2:1 for chemical vapor infiltration for 10-60 h. Through the optimized densification strengthening process, the surface area internal defects generated in the preparation process are favorably repaired, so that the performance of the winding formed carbon/carbon composite material is further improved.
Compared with the prior art, the invention has the following advantages:
1. the invention firstly prepares the winding body with the thickness larger than that of the target product revolution body type carbon/carbon composite material, and then introduces the asphalt and adopts the external shaping internal pressurization heat treatment process and the strengthening process until the thickness of the winding body reaches the target product thickness, thereby increasing the volume content of carbon fibers in the target product revolution body type carbon/carbon composite material, improving the structure of the revolution body type carbon/carbon composite material, improving the performance of the revolution body type carbon/carbon composite material, shortening the densification period in the subsequent process and further improving the preparation efficiency of the revolution body type carbon/carbon composite material.
2. The invention overcomes the defect of low average tension value caused by decreasing tension in the winding process by introducing the asphalt and adopting the internal pressurization heat treatment process of external shaping, improves the winding effect, simultaneously reduces the interlayer spacing of the dipping piece and ensures that the asphalt is uniformly distributed and fully permeated through fiber slippage and asphalt migration in the internal pressurization heat treatment process, effectively inhibits the generation of interlayer and in-layer defects, and improves the quality of the revolution body type carbon/carbon composite material.
3. The invention carries out heat treatment under the internal pressurization state, improves the carbon residue rate of the asphalt, is beneficial to improving the intensity of the asphalt pyrolytic carbon and improving the tight combination degree of the asphalt pyrolytic carbon and fibers, improves the combination property between the revolving body type carbon/carbon composite material layers, further improves the mechanical property and the thermal property of the revolving body type carbon/carbon composite material, meets the application requirements of most structural members, and enlarges the application range of the revolving body type carbon/carbon composite material.
4. The invention solves the problems of slippage, deformation and the like of the carbon/carbon composite material formed by conventional winding under the condition of outer shaping and inner pressurization by carrying out the carbonization and graphitization of progressive gradient pressurization, is beneficial to inhibiting the elliptical deformation of the revolution body type carbon/carbon composite material caused by the uneven change of each component of the material in the carbonization and graphitization processes, ensures the stability of the structural dimension of the product, realizes the near net size manufacturing, reduces the subsequent machining process and further improves the preparation efficiency of the revolution body type carbon/carbon composite material.
5. The invention preferably adopts a step-type external-shaping internal-pressurization heat treatment process and parameters, overcomes the defects of local delamination in the carbonization process of the dipped part after pitch dipping and delamination or cracking caused by volume shrinkage in high-temperature treatment, simultaneously eliminates internal residual stress formed in the subsequent densification strengthening process, and effectively ensures the internal quality and comprehensive performance of the revolved carbon/carbon material product.
6. The invention further improves the density of the carbon/carbon composite material through the subsequent densification strengthening treatment, covers the surface damage and the internal microcracks of the carbon/carbon composite material and further improves the service performance of the carbon/carbon composite material.
7. The revolving body carbon/carbon composite material prepared by the invention has the hoop tensile strength of more than 120MPa, the bending strength of more than 150MPa, the interlaminar shear strength of more than 15MPa, and the thermal expansion coefficient (1000 ℃) of less than 3.0 multiplied by 10-6The solid of revolution carbon/carbon composite material has high overall mechanical and thermophysical properties and good dimensional stability, and simultaneously realizes near-net-size manufacturing, the loss of the preparation raw material is reduced by more than 30 percent, and the density is 1.40g/cm3The preparation period of the carbon/carbon material is shortened to be within 35 days.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a block flow diagram of a preparation method of the present invention.
FIG. 2 is a schematic structural view of a hot press apparatus used for the internal pressure heat treatment of the present invention.
Description of the reference numerals
1-dipping member; 2-pressure transmission medium material; 3-hot pressing auxiliary ring;
4, hot pressing the mold; 5-a heating element; 6-hot pressing head.
Detailed Description
As shown in fig. 1, the preparation method of the present invention comprises the following steps: firstly, preparing a core mould, then winding carbon fibers on the prepared core mould for forming, carrying out vacuum pressure impregnation, carrying out internal pressurization heat treatment for external shaping, and finally carrying out strengthening treatment to obtain the revolving body carbon/carbon composite material.
As shown in fig. 2, the internal pressure heat treatment device adopted by the present invention comprises a hot pressing mold 4 for holding the impregnated member 1, and a heating element 5 arranged outside the hot pressing mold 4, wherein the pressure transmission medium material 2 is distributed inside the impregnated member 1 in the hot pressing mold 4, and the upper end of the impregnated member 1 in the hot pressing mold 4 is provided with a hot pressing auxiliary ring 3, and the hot pressing auxiliary ring 3 is matched with a hot pressing head 6.
Example 1
The preparation method of this example includes the following steps:
step one, core mould preparation: determining the inner diameter of the target product cylindrical carbon/carbon composite material is 660mm, the outer diameter is 690mm, the wall thickness is 30mm, the length is 500mm, the high-temperature elliptical deformation is not more than 3mm, and the density is not less than 1.65g/cm3According to the heat treatment deformation rule of the target product cylindrical carbon/carbon composite material and the adopted continuous carbon fiber, designing a metal core mold with the outer surface shape being the same as the inner surface shape of the target product cylindrical carbon/carbon composite material, the length being 600mm and the outer diameter being 586mm, cleaning the outer surface of the metal core mold by adopting a cleaning agent, then laying polytetrafluoroethylene demolding cloth on the outer surface of the cleaned metal core mold and brushing silicone grease on the polytetrafluoroethylene demolding cloth to be used as a demolding agent;
step two, winding carbon fibers: winding 4 groups of yarns of 12K PAN-based continuous carbon fibers on a metal core mould coated with a silicone release agent in the step one by adopting a winding machine according to a mode of annular spiral alternate winding, wherein the spiral winding angle is 20 degrees, the annular winding angle is 85 degrees, and a winding piece is formed on the metal core mould; in the process of the circumferential and spiral alternate winding, a control host of the winding machine automatically controls a machine head of the winding machine, and the winding direction of the continuous carbon fiber is gradually and automatically converted into the circumferential winding direction from the spiral winding direction or gradually and automatically converted into the spiral winding direction from the circumferential winding direction under the condition of not cutting off the continuous carbon fiber so as to realize the continuous transition between the spiral winding layer and the circumferential winding layer; the winding adopts an equal tension winding mode, and the tension is 42N; the dimensions of the wrapping are: the inner diameter is 586mm, the outer diameter is 691mm, the thickness is 52.5mm, the height is 520mm, and the fiber volume content Vf in the winding piece is 55%;
step three, vacuum pressure impregnation: embedding the winding piece obtained in the step two and the metal core mold into medium temperature asphalt, then placing the winding piece and the metal core mold into a sleeve of a vacuum pressure impregnation furnace for vacuum pressure impregnation, and performing internal and external surface machining treatment after demolding to obtain an impregnated piece with the outer diameter of 690 mm; the vacuum pressure impregnation process comprises the following steps: under the condition of nitrogen atmosphere, heating to 320 ℃ within 80min, vacuumizing to 0.092MPa and keeping for 2h, introducing nitrogen, pressurizing to 2MPa and keeping for 2 h;
step four, internal pressurization heat treatment: placing the impregnated part obtained in the third step in a hot-pressing die 1 of a hot-pressing device, applying a shaping tool (namely a hot-pressing auxiliary ring 3) on the outer surface of the impregnated part, placing a pressure transmission medium material 2 in the impregnated part, pressurizing graphite powder serving as the pressure transmission medium material 2 by a hot-pressing head 6 under the condition of nitrogen atmosphere, heating and raising the temperature by a heating body 5, and performing internal pressure heat treatment on the impregnated part and the hot-pressing auxiliary ring 3 to simultaneously increase the inner diameter and the outer diameter of the impregnated part and ensure that the increase value of the outer diameter is smaller than the increase value of the inner diameter, so that the thickness of the impregnated part is reduced, and a cylindrical carbon/carbon composite material blank is obtained; the inner diameter of the hot-pressing die 1 is 691 mm; the internal pressure heat treatment process comprises the following steps: (1) firstly, heating to 150 ℃ at the speed of 20-35 ℃/min under the pressure of 4-8 MPa; (2) then heating to 320 ℃ at the speed of 10-35 ℃/min under the pressure of 4-8 MPa, and preserving heat for 3 h; (3) continuously heating to 400 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and keeping the temperature for 0.5 h; (4) continuously heating to 550 ℃ at the speed of 1-3 ℃/min under the pressure of 4-8 MPa, and keeping the temperature for 0.5 h; (5) continuously heating to 900 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and preserving heat for 1h to finish carbonization; the sizes of the carbonized impregnation piece are as follows: inner diameter 658mm, outer diameter 690.5mm, thickness 16.25mm, height 520mm,the fiber volume content Vf in the carbonized impregnation member is 65%; (6) in a graphitization furnace, under the pressure of 2MPa, graphite powder is used as a pressure transfer medium for internal pressurization graphitization treatment, the temperature is raised to 2600 ℃ at the speed of 50 ℃/min, the heat is preserved for 1h to complete graphitization, and then the furnace is cooled to room temperature; the thickness of the cylindrical carbon/carbon composite material blank is 30mm, the average value Vf of the volume content of the fibers is 75%, the number of layers is 65 layers/cm, and the density is 1.45g/cm3No obvious layering and other defects;
step five, strengthening treatment: and C, mechanically processing the cylindrical carbon/carbon composite material blank obtained in the fourth step, then placing the cylindrical carbon/carbon composite material blank in a chemical vapor infiltration furnace, vacuumizing the chemical vapor infiltration furnace to 500Pa, heating the cylindrical carbon/carbon composite material blank to 950 ℃ at the speed of 100-300 ℃/h, keeping the vacuum degree in the chemical vapor infiltration furnace lower than 2000Pa, and then introducing argon and natural gas into the chemical vapor infiltration furnace according to the volume ratio of 2:1 for chemical vapor infiltration for 10 hours for strengthening to obtain the cylindrical carbon/carbon composite material.
The density of the cylindrical carbon/carbon composite material prepared in the example is 1.66g/cm3The high-temperature elliptical deformation does not exceed 2mm, the machining performance is good, the hoop tensile strength is 200MPa, the interlaminar shear strength is 27MPa, and the carbon/carbon composite material in the shape of a cylinder has no obvious defects of layering and the like.
The continuous carbon fiber in the second step of this embodiment may also be one or more than two of PAN-based carbon fiber, pitch-based carbon fiber and viscose-based carbon fiber other than PAN-based continuous carbon fiber.
In the fifth embodiment, the strengthening treatment method may also adopt liquid-phase resin impregnation and carbonization, chemical vapor deposition or brush coating.
Example 2
The preparation method of this example includes the following steps:
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 not less than 1.45g/cm3The interlayer bonding strength is not less than 15MPa, the circumferential tensile strength index is not less than 120MPa, the core mold is made of electrode graphite, and the outer diameter of the core mold is 597 mm; step two, spiral windingThe winding angle is 85 degrees, the circumferential winding angle is 87 degrees, the inner diameter of the winding piece is 597mm, the outer diameter is 660mm, and the thickness is 31.5 mm; in the fourth step, the inner diameter of the hot-pressing die is 670mm, the gap between the hot-pressing die and the winding piece is 5mm, and the process of the internal pressurization heat treatment comprises the following steps: (1) firstly, heating to 150 ℃ at the speed of 20-35 ℃/min under the pressure of 4-8 MPa; (2) then heating to 320 ℃ at the speed of 10-35 ℃/min under the pressure of 4-8 MPa, and preserving heat for 1 h; (3) continuously heating to 400 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and preserving heat for 2 h; (4) continuously heating to 550 ℃ at the speed of 1-3 ℃/min under the pressure of 4-8 MPa, and preserving heat for 2 h; the thickness of the carbon/carbon crucible side green body is 30mm, the average value Vf of the fiber volume content is 68%, the number of layers is 50 layers/cm, and the density is 1.45g/cm3No obvious layering and other defects; and fifthly, obtaining the carbon/carbon crucible side green body, wherein the chemical vapor infiltration temperature is 1300 ℃, and the chemical vapor infiltration time is 60 hours.
The detection proves that the density of the carbon/carbon crucible edge prepared in the embodiment is 1.57g/cm3The high-temperature elliptical deformation does not exceed 2mm, the machining performance is good, the hoop tensile strength is 178MPa, the interlaminar shear strength is 25MPa, and the carbon/carbon crucible side has no obvious defects of layering and the like.
Example 3
The preparation method of this example includes the following steps:
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 not less than 1.55g/cm3The interlayer bonding strength is not less than 22MPa, the circumferential tensile strength index is not less than 170MPa, the core mold is made of electrode graphite, and the outer diameter of the core mold is 609 mm; in the second step, the spiral winding angle is 55 degrees, the annular winding angle is 89 degrees, the inner diameter of a winding piece is 609mm, the outer diameter is 690mm, and the thickness is 40.5 mm; in the fourth step, the inner diameter of the hot-pressing die is 696mm, the gap between the hot-pressing die and the winding piece is 3mm, and the internal pressurization heat treatment process comprises the following steps: (1) firstly, heating to 150 ℃ at the speed of 20-35 ℃/min under the pressure of 4-8 MPa; (2) then heating to 320 ℃ at the speed of 10-35 ℃/min under the pressure of 4-8 MPa, and preserving heat for 2 h; (3) continuously under the pressure of 4 MPa-8 MPa and at the temperature of 5 DEG CHeating to 400 ℃ at the speed of/min-10 ℃/min and preserving heat for 1.2 h; (4) continuously heating to 550 ℃ at the speed of 1-3 ℃/min under the pressure of 4-8 MPa, and preserving heat for 1.2 h; the thickness of the cylindrical carbon/carbon composite material blank is 30mm, the average value Vf of the volume content of the fibers is 70%, the number of layers is 55 layers/cm, and the density is 1.55g/cm3No obvious layering and other defects; and fifthly, obtaining the carbon/carbon crucible side, wherein the chemical vapor infiltration temperature is 1130 ℃, and the chemical vapor infiltration time is 35 hours.
The detection proves that the density of the carbon/carbon crucible edge prepared in the embodiment is 1.57g/cm3The high-temperature elliptical deformation does not exceed 2mm, the machining performance is good, the hoop tensile strength is 178MPa, the interlaminar shear strength is 25MPa, and the carbon/carbon crucible side has no obvious defects of layering and the like.
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 (11)
1. The preparation method of the revolving body carbon/carbon composite material is characterized by comprising the following steps:
step one, core mould preparation: cleaning the outer surface of the core mold by using a cleaning agent, then laying release cloth on the outer surface of the cleaned core mold, and brushing a release agent on the release cloth;
step two, winding carbon fibers: winding the continuous carbon fiber on the core mold coated with the release agent in the step one by using a winding machine, and forming a winding piece on the core mold; the thickness of the winding piece is larger than that of the target product revolution body type carbon/carbon composite material;
step three, vacuum pressure impregnation: embedding the winding piece obtained in the step two and the core mold into asphalt, then placing the winding piece and the core mold into a vacuum pressure impregnation furnace for vacuum pressure impregnation, and performing internal and external surface machining treatment after demolding to obtain an impregnated piece;
step four, internal pressurization heat treatment: applying a shaping tool to the outer surface of the impregnated part obtained in the third step, putting or introducing a pressure transmission medium material into the impregnated part, and then carrying out internal pressurization heat treatment on the impregnated part and the shaping tool through the pressure transmission medium material to simultaneously increase the inner diameter and the outer diameter of the impregnated part and ensure that the increase value of the outer diameter is smaller than the increase value of the inner diameter, so that the thickness of the impregnated part is reduced, and a revolved body carbon/carbon composite material blank is obtained; the internal pressure heat treatment process comprises the following steps: pressurizing the dipping part internally, carrying out heat treatment on the dipping part and the shaping tool, increasing the pressure and maintaining the pressure when the temperature of the heat treatment is raised to the asphalt softening temperature in the dipping part, and then raising the temperature in a pressure maintaining state to sequentially carry out carbonization and graphitization; the thickness of the revolution body carbon/carbon composite material blank is not less than that of the revolution body carbon/carbon composite material of the target product;
step five, strengthening treatment: strengthening the rotator type carbon/carbon composite material blank obtained in the fourth step to obtain a rotator type carbon/carbon composite material; the strengthening method is densification treatment or/and coating preparation treatment, wherein the densification treatment adopts resin liquid-phase impregnation carbonization or chemical vapor infiltration, and the coating preparation treatment adopts chemical vapor deposition or brush coating.
2. The method for preparing a revolved body type carbon/carbon composite material according to claim 1, wherein the shape of the outer surface of the core mold in the first step is the same as or similar to the shape of the inner surface of the revolved body type carbon/carbon composite material as a target product.
3. The method for preparing a carbon/carbon composite material as claimed in claim 1, wherein the continuous carbon fiber in the second step is one or more of PAN-based carbon fiber, pitch-based carbon fiber and viscose-based carbon fiber.
4. The method for preparing a revolving body type carbon/carbon composite material according to claim 1, wherein the winding manner in the second step is spiral winding or circumferential spiral alternate winding, wherein the circumferential winding angle is 85 to 89 degrees, the spiral winding angle is 20 to 85 degrees, and in the circumferential spiral alternate winding process, the machine head of the winding machine is automatically controlled by a control host of the winding machine, so that the winding direction of the continuous carbon fiber is gradually and automatically converted from the spiral winding direction to the circumferential winding direction or from the circumferential winding direction to the spiral winding direction under the condition of not cutting the continuous carbon fiber, so as to realize the continuous transition between the spiral winding layer and the circumferential winding layer.
5. The method for preparing the revolving body type carbon/carbon composite material according to claim 1, wherein the thickness of the winding piece in the second step is 1.05 to 1.75 times of the thickness of the revolving body type carbon/carbon composite material obtained in the fifth step.
6. The method for preparing revolved body type carbon/carbon composite material according to claim 1, characterized in that in step four, the average value Vf of the fiber volume content in the revolved body type carbon/carbon composite material blank is more than 65% or the layer number distribution is not less than 50 layers/cm.
7. The method for preparing a revolving body type carbon/carbon composite material according to claim 1, wherein in the fourth step, the inner diameter of the sizing tool is larger than the outer diameter of the impregnated member, and the size of the gap between the sizing tool and the impregnated member is 0.5mm to 5 mm.
8. The method for preparing a revolving body type carbon/carbon composite material according to claim 1, characterized in that the pressure-transmitting medium material used for the carbonization and graphitization in step four is a solid phase, and the pressure-transmitting medium material of the solid phase is graphite powder or silicon powder for carbonization.
9. The method for preparing a revolving body type carbon/carbon composite material according to claim 1, wherein the internal pressurization heat treatment in step four is performed under vacuum or inert atmosphere protection, and the carbonization and graphitization both adopt a step heating heat treatment process.
10. The method for preparing a revolving body type carbon/carbon composite material according to claim 1, wherein the internal pressure heat treatment in step four is by the following rule: (1) firstly, heating to the asphalt softening temperature at the speed of 20-35 ℃/min under the pressure of 4-8 MPa; (2) then heating to the temperature of the lowest viscosity value of the asphalt at the speed of 10-35 ℃/min under the pressure of 4-8 MPa, and preserving the heat for 1-3 h; (3) continuously heating to 400 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and keeping the temperature for 0.5-2 h; (4) continuously heating to 550 ℃ at the speed of 1-3 ℃/min under the pressure of 4-8 MPa, and keeping the temperature for 0.5-2 h; (5) continuously heating to 900 ℃ at the speed of 5-10 ℃/min under the pressure of 4-8 MPa, and preserving the temperature for 1-2 h to finish carbonization; (6) heating to 2600 deg.C at the speed of 5-50 deg.C/min under the pressure of 2-5 MPa, maintaining for 1-2 h to complete graphitization, and cooling to room temperature along with the furnace.
11. The method for preparing a revolving body type carbon/carbon composite material according to claim 1, wherein the specific process of chemical vapor infiltration strengthening in the step five is as follows: vacuumizing the chemical vapor infiltration furnace, heating to 950-1300 ℃ at the speed of 100-300 ℃/h, keeping the vacuum degree in the chemical vapor infiltration furnace lower than 2000Pa, and introducing inert gas and hydrocarbon gas into the chemical vapor infiltration furnace according to the volume ratio of 2:1 for chemical vapor infiltration for 10-60 h.
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