CN116283334A - C/C composite material connection method - Google Patents

C/C composite material connection method Download PDF

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CN116283334A
CN116283334A CN202211690548.4A CN202211690548A CN116283334A CN 116283334 A CN116283334 A CN 116283334A CN 202211690548 A CN202211690548 A CN 202211690548A CN 116283334 A CN116283334 A CN 116283334A
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composite material
sub
carbon fiber
connecting piece
connector
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王芙愿
朱昊
史思涛
董强
王卿
成来飞
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Xian Xinyao Ceramic Composite Material Co Ltd
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Xian Xinyao Ceramic Composite Material Co Ltd
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    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract

The invention relates to a connecting method of composite materials, in particular to a C/C composite material connecting method, which solves the problems that when complex components are assembled by rivet, bolt and other connecting modes, single rivet and bolt structures have failure modes of rivet fracture, thread tooth fracture and the like, and serious potential safety hazards exist for complex components. The C/C composite material connecting method comprises the following steps: 1) Preparing a carbon matrix of the carbon fiber preform to obtain a carbon fiber preform with a density of 1.2-1.5g/cm 3 Or at least two sub-members and at least one connector; 2) Stirring an organic solvent and silicon powder or silicon alloy powder according to a ratio of 1:2-4, and respectively brushing the surfaces of the joints of at least two subcomponents or at least two subcomponentsAnd at least one connecting part connecting surface, fixing to obtain a C/C composite material connecting part; 3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connector obtained in the step (2), and introducing argon to obtain the C/C composite material connector.

Description

C/C composite material connection method
Technical Field
The invention relates to a connecting method of composite materials, in particular to a connecting method of C/C composite materials.
Background
The C/C composite material is a carbon fiber and fabric reinforced carbon matrix composite material, and has low density<2.0g/cm 3 ) The high-strength high-specific modulus high-thermal conductivity low-expansion coefficient high-friction-performance high-thermal-shock-resistance high-dimensional stability high-temperature heat-resistant material is a few alternative materials applied at a temperature of 1650 ℃ or higher, and the highest theoretical temperature of the material is 2600 ℃, so that the material is considered to be one of the most promising high-temperature materials. The C/C composite material has been widely used in the fields of aerospace, automobile industry, medicine and the like due to the unique performance, such as rocket engine jet pipes and throat liners thereof, thermal protection systems of end caps and wing leading edges of spacecrafts, aircraft brake discs and the like.
At present, the preparation of the complex structural member of the C/C composite material mainly comprises two processes of integral braiding and forming and combined assembly. The fiber integral braiding molding technology is only suitable for manufacturing part of axisymmetric shell components, and the combined assembly molding technology is suitable for manufacturing components with irregular and complex structures, so that the preparation of the current complex components is mainly based on the combined assembly molding technology. Firstly, dividing a complex structural member into a plurality of sub-member-level members, and then assembling the complex structural member by means of rivet, bolt and other connection modes; the method is simple and convenient, but the failure modes of rivet fracture, thread tooth fracture and the like exist in a single rivet and bolt structure, and serious potential safety hazards exist for complex structural members.
Disclosure of Invention
The invention aims to solve the problem that when complex components are assembled in the existing connecting modes such as rivets, bolts and the like, failure modes such as rivet fracture, thread tooth fracture and the like exist in a single rivet and bolt structure, and serious potential safety hazards exist for the complex components, and provides a C/C composite material connecting method.
In order to solve the technical problems, the invention adopts the following technical scheme:
the C/C composite material connecting method is characterized by comprising the following steps of:
1) Preparing a carbon matrix of the carbon fiber preform to obtain a carbon fiber preform with a density of 1.2-1.5g/cm 3 Or at least two sub-members and at least one connector;
2) Stirring an organic solvent and silicon powder or silicon alloy powder according to a mass ratio of 1:2-4, respectively brushing the surfaces of the joints of at least two subcomponents obtained in the step 1), or the surfaces of the joints of at least two subcomponents and at least one connecting piece, and fixing to obtain a C/C composite material connecting piece;
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connector obtained in the step (2), and introducing argon to obtain the C/C composite material connector.
Further, the step 2) specifically comprises:
uniformly stirring the low-concentration resin slurry and silicon powder or silicon alloy powder according to the mass ratio of 1:2-4, respectively uniformly brushing a coating on the surface of the joint of at least two subcomponents obtained in the step 1) or the surface of the joint of at least two subcomponents and at least one connecting piece until the thickness of the coating is 2-3mm, and then fixing the at least two subcomponents obtained in the step 1) or the at least two subcomponents and the at least one connecting piece by using a graphite fixture or carbon fiber to obtain the C/C composite material connecting piece.
Further, in the step 2), the low-concentration resin slurry specifically includes:
the low-concentration resin comprises 20-30% of phenolic resin and 70-80% of absolute ethyl alcohol by mass.
Further, in step 2), the connection mode of the at least two sub-components, or the at least two sub-components and the at least one connecting piece, is specifically:
the at least two sub-components are connected in a planar fit manner; or at least two sub-components are connected in a way of matching grooves and projections;
or the connecting piece is a pin, and at least two sub-components are connected in a plane joint pin fixing mode.
Further, the step 1) specifically comprises:
preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with a density of 1.2-1.5g/cm 3 Or at least two sub-members and at least one connector.
Further, the step 3) specifically comprises:
and (3) carrying out high-temperature in-situ reaction on the C/C composite material connecting piece in the step (2) at 1400-1700 ℃, introducing argon for protection in the whole process, and reacting for 0.5-2h to obtain the C/C composite material connecting body.
Further, in the step 3), the high-temperature in-situ reaction specifically includes:
vacuumizing the vacuum tube furnace, heating to 1000 ℃ according to the heating condition of 10 ℃/min, preserving heat for 0.5h, heating to 1400-1700 ℃ according to the heating condition of 5 ℃/min, preserving heat for 1-2h, and cooling.
Further, in the step 2), the organic solvent and the silicon powder or the silicon alloy powder are stirred according to the mass ratio of 1:3.
Further, step 3) further comprises:
and polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
(1) According to the C/C composite material connecting method, a silicon source (silicon powder or silicon alloy powder) is introduced to the surface of the C/C composite material by adopting a brushing method, and the C/C composite material is connected by adopting a high-temperature in-situ reaction (Si/C in-situ reaction) mode, so that the strength of the obtained C/C composite material connecting piece is higher, the processing difficulty is reduced, and the cost is saved.
(2) The invention discloses a C/C composite material connecting method, which is used for connecting components under different working conditions by designing different structures. When the shearing strength requirement on the C/C composite material is high, riveting (pin connection) and a buckling structure (matching of a groove and a bump) can be adopted for connection. Meanwhile, the riveting structure is simple and easy to process, is suitable for components insensitive to local fiber damage, and the buckling structure is suitable for local fiber damage sensitive structural components, and can form complementary advantages.
(3) According to the C/C composite material connecting method, the C/C composite materials are tightly connected through Si/C in-situ reaction, so that a compact interface layer of silicon carbide coated silicon is formed, the problems of high processing difficulty of a complex carbon ceramic material structural member and high potential safety hazard of a combined structural member can be effectively solved, and the C/C composite material connecting method has a wide application prospect.
Drawings
FIG. 1 is a schematic view of a connection structure of a C/C composite material with high-temperature glue according to a first embodiment of a connection method of a C/C composite material of the present invention;
FIG. 2 is a schematic diagram showing the connection of the pin structures of the C/C composite material in the second embodiment of the connection method of the C/C composite material of the present invention;
FIG. 3 is a schematic view of a C/C composite circular snap-in connection in accordance with a third embodiment of the method of the present invention;
FIG. 4 is a schematic illustration of a fully embedded snap connection of a C/C composite material in a fourth embodiment of a method of connecting a C/C composite material according to the present invention;
FIG. 5 is a schematic illustration of a C/C composite semi-embedded snap-fit connection in a fifth embodiment of a method of connecting a C/C composite of the present invention.
Detailed Description
Example 1
The invention provides a C/C composite material connecting method aiming at different working conditions, and solves the problems of high processing difficulty, unsafe connection and the like of the existing complex C/C structural member by Si/C in-situ reaction connection. The method comprises the following specific steps:
1) Preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with the density of 1.2g/cm 3 Is provided. As shown in fig. 1, the connection surfaces of the two sub-members are planar.
2) Uniformly stirring the low-concentration resin slurry and the silicon powder according to a ratio of 1:2, uniformly brushing a coating on the connecting surfaces of the two sub-components obtained in the step 1), wherein the thickness of the coating is 2-3mm, and the thickness of the coating is 2mm in the embodiment, then fixing the two sub-components obtained in the step 1) by using a graphite fixture or carbon fiber to prevent dislocation of high-temperature reaction, and finally obtaining the C/C composite material connecting piece. In this embodiment, the low-concentration resin is composed of a phenolic resin and absolute ethyl alcohol, wherein the mass percentage of the phenolic resin is 20%, and the mass percentage of the absolute ethyl alcohol is 80%.
The thickness of the coating is controlled to be 2-3mm, mainly because: when the thickness of the coating is less than 2mm, the interface bonding is poor; when the thickness of the coating is more than 3mm, the thickness of the interfacial phase is increased, the brittle phase is increased, and brittle fracture of the interfacial phase is easy to occur.
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connector in the step (2) at 1400 ℃, introducing argon for protection in the whole process, and reacting for 2h to obtain the C/C composite material connector. And finally, polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
The high-temperature in-situ reaction is to vacuumize a vacuum tube furnace, then heat up to 1000 ℃ according to the heating condition of 10 ℃/min, heat preservation for 0.5h, then heat up to 1400-1700 ℃ according to the heating condition of 5 ℃/min, heat preservation for 1-2h, and then cool along with the vacuum tube furnace. Wherein, the heat preservation can better promote the carbonization process of the resin under the condition of 1000 ℃.
For load bearing components, such as aerospace component support portions and the like; because the shearing force is not strictly required, only the surfaces of the two sub-component connectors are polished to be rough, and then the connection is carried out.
Example two
1) Preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with a density of 1.3g/cm 3 And two connectors. As shown in fig. 2, in this embodiment, the connection surfaces of the two sub-members are planar, and the two connection members are two pins.
2) Uniformly stirring the low-concentration resin slurry and silicon powder or silicon alloy powder according to a ratio of 1:3, and uniformly brushing a coating on the connecting surfaces of the two sub-components and the connecting surfaces of the two pins obtained in the step 1) until the thickness of the coating is 3mm. And then fixing the two sub-components obtained in the step 1) by using a graphite clamp or carbon fiber to prevent dislocation of high-temperature reaction, and finally connecting by using two pins to obtain the C/C composite material connecting piece. In this embodiment, the low-concentration resin is composed of a phenolic resin and absolute ethyl alcohol, wherein the mass percentage of the phenolic resin is 25%, and the mass percentage of the absolute ethyl alcohol is 75%.
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connector in the step (2) at 1500 ℃, introducing argon for protection in the whole process, and reacting for 1h to obtain the C/C composite material connector. And finally, polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
For layer shear components, such as brake discs and the like, large shearing force is applied in the use process, so that strict requirements are placed on interlayer shearing inside the C/C composite material connector. Such components are connected according to the pin configuration of fig. 2.
Example III
1) Preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with a density of 1.4g/cm 3 As shown in fig. 3, two circular grooves are provided on one of the sub-member connection surfaces, and two circular protrusions matching the grooves are provided on the other sub-member connection surface at positions corresponding to the grooves.
2) Uniformly stirring the low-concentration resin slurry and silicon powder or silicon alloy powder according to a ratio of 1:4, uniformly coating the connecting surfaces of the two sub-components obtained in the step 1) with a coating until the thickness of the coating is 2mm, fixing the two sub-components obtained in the step 1) by using a graphite clamp or carbon fiber, preventing the dislocation of high-temperature reaction, and finally obtaining the C/C composite material connecting piece. In this embodiment, the low-concentration resin is composed of a phenolic resin and absolute ethyl alcohol, wherein the mass percentage of the phenolic resin is 30%, and the mass percentage of the absolute ethyl alcohol is 70%.
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connecting piece in the step (2) at 1600 ℃, introducing argon for protection in the whole process, and reacting for 1h to obtain the C/C composite material connecting body. And finally, polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
The circular buckle type connecting structure shown in fig. 3 is still suitable for layer shear type components, and the damage of fibers can be reduced to a certain extent.
Example IV
1) Preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with the density of 1.5g/cm 3 As shown in fig. 4, a groove is formed on one of the sub-member connection surfaces, and a projection adapted to the groove is formed on the other sub-member connection surface at a position corresponding to the groove.
2) Uniformly stirring the low-concentration resin slurry and silicon powder or silicon alloy powder according to a ratio of 1:3, uniformly coating the connecting surfaces of the two sub-components obtained in the step 1) with a coating until the thickness of the coating is 2mm, fixing the two sub-components obtained in the step 1) by using a graphite clamp or carbon fiber, preventing the dislocation of high-temperature reaction, and finally obtaining the C/C composite material connecting piece. In this embodiment, the low-concentration resin is composed of a phenolic resin and absolute ethyl alcohol, wherein the mass percentage of the phenolic resin is 28%, and the mass percentage of the absolute ethyl alcohol is 72%.
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connecting piece in the step (2) at 1700 ℃, introducing argon for protection in the whole process, and reacting for 0.5h to obtain the C/C composite material connecting body. And finally, polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
The fully embedded snap connection structure shown in fig. 4 is still suitable for use with layer shear type members for members that are subject to large interlaminar shear forces.
Example five
1) Preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with a density of 1.45g/cm 3 As shown in fig. 5, two grooves penetrating in the width direction are formed in one of the sub-member connection surfaces, and two protrusions matching with the grooves are formed in the other sub-member connection surface at positions corresponding to the grooves.
2) Uniformly stirring the low-concentration resin slurry and silicon powder or silicon alloy powder according to a ratio of 1:3, uniformly coating the connecting surfaces of the two sub-components obtained in the step 1) with a coating until the thickness of the coating is 2mm, fixing the two sub-components obtained in the step 1) by using a graphite clamp or carbon fiber, preventing the dislocation of high-temperature reaction, and finally obtaining the C/C composite material connecting piece. In this embodiment, the low-concentration resin is composed of a phenolic resin and absolute ethyl alcohol, wherein the mass percentage of the phenolic resin is 23%, and the mass percentage of the absolute ethyl alcohol is 77%.
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connecting piece in the step (2) at 1700 ℃, introducing argon for protection in the whole process, and reacting for 1h to obtain the C/C composite material connecting body. And finally, polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
The semi-embedded buckle connection structure shown in fig. 5 is still suitable for layer shear type components, and the use safety of the connection components can be better ensured.

Claims (9)

1. A method for connecting a C/C composite material, comprising the steps of:
1) Preparing a carbon matrix of the carbon fiber preform to obtain a carbon fiber preform with a density of 1.2-1.5g/cm 3 Or at least two sub-members and at least one connector;
2) Stirring an organic solvent and silicon powder or silicon alloy powder according to a mass ratio of 1:2-4, respectively brushing the surfaces of the joints of at least two subcomponents obtained in the step 1), or the surfaces of the joints of at least two subcomponents and at least one connecting piece, and fixing to obtain a C/C composite material connecting piece;
3) And (3) carrying out high-temperature in-situ reaction on the C/C composite material connector obtained in the step (2), and introducing argon to obtain the C/C composite material connector.
2. The method for connecting C/C composite materials according to claim 1, wherein step 2) comprises:
uniformly stirring the low-concentration resin slurry and silicon powder or silicon alloy powder according to the mass ratio of 1:2-4, respectively uniformly brushing a coating on the surface of the joint of at least two subcomponents obtained in the step 1) or the surface of the joint of at least two subcomponents and at least one connecting piece until the thickness of the coating is 2-3mm, and then fixing the at least two subcomponents obtained in the step 1) or the at least two subcomponents and the at least one connecting piece by using a graphite fixture or carbon fiber to obtain the C/C composite material connecting piece.
3. The method for joining C/C composite materials according to claim 2, wherein in step 2), the low-concentration resin paste is specifically:
the low-concentration resin comprises 20-30% of phenolic resin and 70-80% of absolute ethyl alcohol by mass.
4. A method for joining C/C composite materials according to claim 3, characterized in that in step 2), the joining means of the at least two sub-components, or of the at least two sub-components and the at least one joining element, are in particular:
the at least two sub-components are connected in a planar fit manner; or at least two sub-components are connected in a way of matching grooves and projections;
or the connecting piece is a pin, and at least two sub-components are connected in a plane joint pin fixing mode.
5. The method for connecting C/C composite materials according to claim 4, wherein step 1) comprises:
preparing a carbon matrix of the carbon fiber preform by adopting a CVI or PIP method to obtain a carbon fiber preform with a density of 1.2-1.5g/cm 3 Or at least two sub-members and at least one connector.
6. The method for joining C/C composite materials according to any one of claims 1 to 5, wherein step 3) comprises:
and (3) carrying out high-temperature in-situ reaction on the C/C composite material connecting piece in the step (2) at 1400-1700 ℃, introducing argon for protection in the whole process, and reacting for 0.5-2h to obtain the C/C composite material connecting body.
7. The method for joining C/C composite materials according to claim 6, wherein in step 3), the high temperature in situ reaction is specifically:
vacuumizing the vacuum tube furnace, heating to 1000 ℃ according to the heating condition of 10 ℃/min, preserving heat for 0.5h, heating to 1400-1700 ℃ according to the heating condition of 5 ℃/min, preserving heat for 1-2h, and cooling.
8. The method for joining C/C composite materials according to claim 7, wherein in step 2), the organic solvent and the silicon powder or the silicon alloy powder are stirred at a mass ratio of 1:3.
9. The method of claim 8, wherein step 3) further comprises:
and polishing, cleaning and drying the residual scum on the surface of the C/C composite material connector.
CN202211690548.4A 2022-12-27 2022-12-27 C/C composite material connection method Pending CN116283334A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101224993A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 SiC based composite material component and on-line jointing preparation method thereof
CN112430117A (en) * 2020-11-25 2021-03-02 中航复合材料有限责任公司 In-situ reaction connection method for silicon carbide-based composite material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101224993A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 SiC based composite material component and on-line jointing preparation method thereof
CN112430117A (en) * 2020-11-25 2021-03-02 中航复合材料有限责任公司 In-situ reaction connection method for silicon carbide-based composite material

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