CN110937909A - Preparation method of continuous fiber reinforced C/SiC ceramic spring - Google Patents
Preparation method of continuous fiber reinforced C/SiC ceramic spring Download PDFInfo
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Abstract
The invention relates to a preparation method of a continuous fiber reinforced C/SiC ceramic spring.A special mould structure is designed, and the C/SiC ceramic spring is obtained by adopting 3D printing, is cylindrical, has threads on the whole body and is provided with through holes distributed among the threads, and is divided into three sections along the axial direction, wherein the middle mould is longer than the ceramic moulds at the two ends; the die is used for preparing a spring preform, the spring preform is toughened by a chemical vapor infiltration method, and a SiC matrix and a coating are deposited on the spring preform. The shear strength of the spring wire is regulated and controlled from the weaving structure design of the carbon fiber, so that the designability of the resilience force, the spring stiffness and the like of the spring is realized; controllability of spring resilience, spring stiffness, fatigue resistance and the like is further realized through uniform interface layers and coating thicknesses which can be accurately controlled; the rigidity retention rate of the ceramic matrix composite spring prepared by the invention at 1000 ℃ can reach 97.6 percent, in particular to the treatment of reinforcement, toughening, molding and the like of carbon fibers, and the ceramic matrix composite spring is mainly applied to the field of high-temperature sliding sealing.
Description
Technical Field
The invention belongs to a preparation method of a spring, relates to a preparation method of a continuous fiber reinforced C/SiC ceramic spring, and particularly relates to a preparation method of a continuous fiber reinforced ceramic matrix composite spring with a designable woven structure, which is mainly applied to the field of high-temperature sliding sealing.
Background
Hypersonic aircrafts refer to winged or wingless aircrafts such as airplanes, missiles, shells and the like with flight speed more than 5 times of sound speed. In order to realize the high-performance work in a wide speed and height range of the whole flight profile, the structure of an air inlet (tail nozzle) needs to be continuously adjusted, and engines such as a rocket-based combined cycle (RBCC) generally adopt a variable geometry air inlet scheme; the variable geometry air inlet channel can increase the weight and the structural complexity of an engine, and can also bring about the problems of sealing, connection, cooling, control and the like, and the variable flow channel ultra-high temperature dynamic sealing is one of the core technologies which need to be solved urgently. In the three main sealing technologies at the present stage, the ceramic chip seal has excellent high temperature resistance and wear resistance, and the sealing performance is also good, so that the application requirements can be better met. An important breakthrough point in ceramic wafer sealing technology is the spring.
In the aspect of high-temperature alloy springs, the nickel-cobalt alloy therm600 in the U.S. can resist high temperature of 500 ℃, the Inconel X750 can resist high temperature of 600 ℃, but the strength and the stability of the alloy are obviously reduced when the temperature exceeds 1000 ℃. Extensive research has been conducted in Japan for the preparation of high temperature resistant composite springs, and Japanese spring corporation (NHK) has successfully developed partially stabilized zirconia, Si3N4The ceramic spring product as the matrix has the maximum use temperature reaching 800 ℃ and 1200 ℃ respectively. The Nanjing university of industry discloses a ceramic spring with Partially Stabilized Zirconia (PSZ) obtained by machining in Chinese patent CN 102757221A, and discloses a method for toughening the spring by using nano particles in Chinese patent CN 1472448A, but the ceramic spring has high brittleness and is added with nano particlesThe labor is difficult. The national defense science and technology university discloses that a spring preform is prepared by adopting a die-casting molding process in Chinese patent CN 102584307A, the spring preform is densified by a precursor conversion process, a SiC oxidation resistant coating is deposited by adopting a CVD process, and the unidirectional carbon fiber reinforced silicon carbide (1D C/SiC) ceramic matrix composite spring is prepared.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of a continuous fiber reinforced C/SiC ceramic spring, which obtains designability of resilience force, spring stiffness and the like of the C/SiC ceramic spring from designability of a carbon fiber weaving structure, a spring forming die to mechanical parameters of the spring; controllability of spring resilience, spring stiffness, fatigue resistance and the like is obtained through controllability of the PyC interface layer and the SiC substrate and the coating which are integrally deposited later; the net forming of the whole process is realized from the net forming of the 3D printing spring die to the net forming of the C/SiC ceramic spring.
Technical scheme
A preparation method of a continuous fiber reinforced C/SiC ceramic spring is characterized by comprising the following steps:
step 1, preparing a spring forming die: according to mechanical design parameters required by the spring, a cylindrical ceramic die which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing; the die is hollow cylindrical and is divided into three sections along the axial direction, and the middle die is longer than the two end dies;
step 2, preparing a spring preform: fixing the three-section die by using a graphite clamp, weaving a plurality of strands of 1K, 3K or 12K carbon fibers into a carbon fiber rope, winding the carbon fiber rope on the die along threads on the whole body of the die, and fixing two ends of the carbon fiber rope to obtain a spring preform;
step 3, toughening the spring preform: placing the spring preform into a deposition furnace, decomposing the spring preform by adopting a chemical vapor infiltration method and taking propylene as an air source under the conditions of 850-1000 ℃ and 0.20-0.25 MPa of pressure in the furnace, and preparing pyrolytic carbon layers on the surface and inside of the preform;
step 4, depositing the SiC matrix and the coating on the spring preform: placing the spring preform processed in the step 3 into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as carrier gas, argon as diluent gas and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 950-1100 ℃ and the pressure in the furnace of 0.09-0.1 MPa, and depositing the SiC in the preform and on the surface of the preform to form a matrix and a coating;
step 5, demolding: and removing the graphite clamps at the two ends of the mold, drawing out the inner mold, converging the outer mold, and drawing out the outer mold from the spring to obtain the C/SiC composite material spring.
The number of strands of the carbon fibers and the number of each strand are determined by the wire diameter of the spring wire required by the spring and the weaving method.
The carbon fiber is woven into the carbon fiber rope by twisting the fibers or weaving the fibers in a mode of 1D, 2D or 3D.
The pyrolytic carbon layer in the step 3 is a PyC or BN interface layer.
Advantageous effects
The invention provides a preparation method of a continuous fiber reinforced C/SiC ceramic spring, which is a preparation method of a continuous fiber reinforced ceramic matrix composite spring with a designable weaving structure, wherein the rigidity retention rate of the spring at 1000 ℃ can reach 97.6 percent, and the preparation method particularly relates to the treatment of reinforcement, toughening, molding and the like of carbon fibers, and is mainly applied to the field of high-temperature sliding sealing. The method is technically characterized in that a special mould structure is designed, a cylindrical mould which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained by adopting 3D printing, the cylindrical mould is divided into three sections along the axial direction, and a middle mould is longer than ceramic moulds at two ends; the die is used for preparing a spring preform, the spring preform is toughened by a chemical vapor infiltration method, and a SiC matrix and a coating are deposited on the spring preform. The technical scheme provided by the invention can regulate and control the shearing strength of the spring wire from the design of the weaving structure of the carbon fiber, and realizes designability of the resilience force, the spring stiffness and the like of the spring; controllability of spring resilience, spring stiffness, fatigue resistance and the like is further realized through uniform interface layers and coating thicknesses which can be accurately controlled; the net shape of the spring is achieved by a reusable mold. The rigidity retention rate of the ceramic matrix composite spring prepared by the invention at 1000 ℃ can reach 97.6 percent, in particular to the treatment of reinforcement, toughening, molding and the like of carbon fibers, and the ceramic matrix composite spring is mainly applied to the field of high-temperature sliding sealing. The net shape of the spring is achieved by a reusable mold. The process has the advantages of excellent designability, accurate controllability, high efficiency and repeatability, and the prepared composite material spring can still maintain excellent performance in high-temperature and oxidation environments.
The invention has the following beneficial effects:
(1) according to the invention, the carbon fiber preforms with different structures are obtained by designing the weaving mode of the carbon fibers, so that the shear stress borne by the carbon fibers in the spring wire is reduced, part of the shear stress is converted into the tensile stress, the shear strength of the spring wire is effectively improved, and the designability of the resilience force, the spring stiffness and the like of the spring can be realized under the condition that the mechanical parameters are not changed.
(2) According to the invention, the PyC interface layer is deposited on the surface of the spring preform through CVI, and then the SiC substrate and the coating are integrally deposited, so that the process is simple and clear, and the deposited layers have good controllability. Meanwhile, the interface layer and the coating are distributed on the surface of the carbon fiber more uniformly, the thickness can be controlled to be 50nm level more accurately, and controllability of spring resilience, spring stiffness, fatigue resistance and the like is further realized.
(3) The invention creatively combines 3D printing with the design of a spring forming mold capable of being opened and closed, on one hand, ceramic molds with different mechanical parameters are conveniently obtained, on the other hand, three molds are fixed by graphite clamps during preparation, the inner mold is pulled out during demolding, and two parts of the outer mold are jointed, so that the net forming of the continuous fiber reinforced ceramic matrix composite springs with different performance parameters can be realized, and the molds can be repeatedly utilized; meanwhile, the whole process is simple and clear, and the repeatability is high.
The spring prepared by the invention is subjected to normal temperature and high temperature of 1000 ℃ elasticity performance tests, and the result shows that: the rigidity retention rate of the spring at 1000 ℃ can reach 97.6%. In general, the preparation process has excellent designability, accurate controllability and high-efficiency repeatability, and the prepared composite material spring can still keep excellent performance under high-temperature and oxidation environments.
Drawings
FIG. 1 is a process flow diagram of the present invention
FIG. 2 is a partial spring pictorial representation of an embodiment of the present invention
FIG. 3 is a pyrolytic carbon layer deposited on the surface of carbon fiber in example 1 of the invention
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the embodiment of the invention adopts the following technical scheme:
step 1. preparation of spring forming die
According to the mechanical design parameters required by the spring, the cylindrical ceramic die which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing. The design concept of the die is mainly divided into two major aspects, on one hand, in order to ensure the smooth demoulding of the spring and the repeated utilization of the die, the die is divided into three parts along the axial direction, the dies on the two sides are provided with threads, through holes are distributed between the threads, the die in the middle part is longer than the other two parts for facilitating drawing and pulling, the side surface is not provided with the threads, and only the through holes distributed according to a spiral line are arranged; on the other hand, in order to ensure the stability of the mechanical parameters of the spring and the sufficiency of the deposition process, the whole die is designed into a hollow cylinder, threads are designed to fix carbon fibers, and through holes between the threads of the dies on two sides, on the side surface of the die in the middle and at the drawing part are designed.
Step 2. preparation of spring preform
Weaving a plurality of strands (such as 16 strands) of 3K bundles of carbon fibers into carbon fiber ropes according to a designed structure, winding the carbon fiber ropes on a die along threads, fixing three dies by using graphite clamps (a layer of graphite paper is stacked between the three dies to be more beneficial to pushing, pulling and pulling), and fixing two ends of the carbon fiber ropes;
step 3, toughening the spring preform
And (2) putting the spring preform in the step (1) into a deposition furnace, decomposing at 850 ℃ by adopting a chemical vapor infiltration method and taking propylene as a gas source, and preparing a pyrolytic carbon (PyC) layer (with the thickness of about 200 nm) on the surface and inside of the preform.
Step 4, depositing SiC matrix and coating on the spring preform
And (3) putting the spring preform obtained in the step (2) into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as a carrier gas, argon as a diluent gas, and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 1000 ℃, 5kPa and 0.01MPa in the furnace, and depositing the SiC in the preform and on the surface of the preform to form a substrate and a coating.
Step 5, demoulding
And removing the graphite clamps at the two ends of the mold, drawing out the inner mold, converging the outer mold, and drawing out the outer mold from the spring to obtain the C/SiC composite material spring.
The specific embodiment is as follows:
example 1.
A spring made of a ceramic matrix composite material according to the present invention as shown in FIG. 2(a) has a stiffness of 2.254N/mm at room temperature and a stiffness of 2.120N/mm in 1000 ℃ air, and has a retention rate of stiffness of about 97.6%.
The method comprises the following steps: preparation of spring forming die
According to a mechanical design manual, mechanical design parameters of the spring shown in the table 1 are designed, and a cylindrical ceramic mold which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing. The design concept of the die is mainly divided into two major aspects, on one hand, in order to ensure the smooth demoulding of the spring and the repeated utilization of the die, the die is divided into three parts along the axial direction, the dies on the two sides are provided with threads, through holes are distributed between the threads, the die in the middle part is longer than the other two parts for facilitating drawing and pulling, the side surface is not provided with the threads, and only the through holes distributed according to a spiral line are arranged; on the other hand, in order to ensure the stability of the mechanical parameters of the spring and the sufficiency of the deposition process, the whole die is designed into a hollow cylinder, threads are designed to fix carbon fibers, and through holes between the threads of the dies on two sides, on the side surface of the die in the middle and at the drawing part are designed.
Step two: and preparing a spring preform. Twisting 16 strands of 3K bundles of carbon fibers with the twist degree of 100 twists/m to form a carbon fiber rope with the diameter of about 2 mm; winding the carbon fiber rope on a die along threads, fixing the three dies by using a graphite clamp, and fixing two ends of the carbon fiber rope;
step three: and (4) toughening the spring preform. And (3) putting the spring preform obtained in the step one into a deposition furnace, decomposing at 850 ℃ by adopting a chemical vapor infiltration method and taking propylene as a gas source, and preparing a pyrolytic carbon (PyC) layer with the thickness of about 200nm on the surface and inside of the preform, as shown in figure 3.
Step four: and depositing the SiC substrate and the coating on the spring preform. And (3) putting the spring preform obtained in the step (2) into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as a carrier gas, argon as a diluent gas, and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 1000 ℃, 5kPa and 0.01MPa in the furnace, and depositing the SiC in the preform and on the surface of the preform to form a substrate and a coating.
Step five: and (6) demolding. Removing graphite clamps at two ends of the mold, drawing out the mold core, converging the external mold, drawing out the mold core from the interior of the spring to obtain the C/SiC composite material spring, wherein the density is 2.000 +/-0.05 g/cm measured according to an Archimedes drainage method3。
Example 2.
A spring of the present invention, as shown in FIG. 2(b), has a stiffness of 2.276N/mm at room temperature.
The method comprises the following steps: preparation of spring forming die
According to a mechanical design manual, mechanical design parameters of the spring shown in the table 1 are designed, and a cylindrical ceramic mold which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing. The design concept of the die is mainly divided into two major aspects, on one hand, in order to ensure the smooth demoulding of the spring and the repeated utilization of the die, the die is divided into three parts along the axial direction, the dies on the two sides are provided with threads, through holes are distributed between the threads, the die in the middle part is longer than the other two parts for facilitating drawing and pulling, the side surface is not provided with the threads, and only the through holes distributed according to a spiral line are arranged; on the other hand, in order to ensure the stability of the mechanical parameters of the spring and the sufficiency of the deposition process, the whole die is designed into a hollow cylinder, threads are designed to fix carbon fibers, and through holes between the threads of the dies on two sides, on the side surface of the die in the middle and at the drawing part are designed.
Step two: and preparing a spring preform. 16 strands of carbon fibers (Dongli T300) are woven into a three-dimensional hollow tubular structure, the volume fraction of the carbon fibers is 40%, the weaving angle is 22 degrees, the diameter of the weaving rope is 2mm, when the carbon fibers are wound on a die, the width perpendicular to the axial edge of the spring wire is 1.5 +/-0.5 mm, and the width parallel to the axial edge of the spring wire is 4.0 +/-0.5 mm. And thus 3D printed Al of corresponding size2O3And (3) fixing the three dies by using a graphite clamp, winding the carbon fiber rope on the dies along threads, and fixing two ends of the carbon fiber rope.
Step three: and (4) toughening the spring preform. And (3) putting the spring preform obtained in the step one into a deposition furnace, decomposing at 850 ℃ by adopting a chemical vapor infiltration method and taking propylene as a gas source, and preparing pyrolytic carbon (PyC) layers on the surface and inside of the preform, wherein the thickness of the pyrolytic carbon layers is about 300 nm.
Step four: and depositing the SiC substrate and the coating on the spring preform. And (3) putting the spring preform obtained in the step (2) into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as a carrier gas, argon as a diluent gas, and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 1000 ℃, 5kPa and 0.01MPa in the furnace, and depositing the SiC in the preform and on the surface of the preform to form a substrate and a coating.
Step five: and (5) performing anti-oxidation treatment. Continuously placing the spring rough blank obtained in the step three into a deposition furnace to deposit a SiC coating, finally obtaining the C/SiC ceramic spring, and measuring the density to be 2.000 +/-0.05 g/cm according to an Archimedes drainage method3。
Example 3.
The rigidity of the ceramic matrix composite material spring reaches 1.793N/mm at room temperature, the rigidity still reaches 1.171N/mm in air at 1000 ℃, and the rigidity retention rate exceeds 65 percent, as shown in figure 2 (a).
The method comprises the following steps: preparation of spring forming die
According to a mechanical design manual, mechanical design parameters of the spring shown in the table 1 are designed, and a cylindrical ceramic mold which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing. The design concept of the die is mainly divided into two major aspects, on one hand, in order to ensure the smooth demoulding of the spring and the repeated utilization of the die, the die is divided into three parts along the axial direction, the dies on the two sides are provided with threads, through holes are distributed between the threads, the die in the middle part is longer than the other two parts for facilitating drawing and pulling, the side surface is not provided with the threads, and only the through holes distributed according to a spiral line are arranged; on the other hand, in order to ensure the stability of the mechanical parameters of the spring and the sufficiency of the deposition process, the whole die is designed into a hollow cylinder, threads are designed to fix carbon fibers, and through holes between the threads of the dies on two sides, on the side surface of the die in the middle and at the drawing part are designed.
Step two: and preparing a spring preform. Twisting 16 strands of 3K bundles of carbon fibers with the twist degree of 100 twists/m to form a carbon fiber rope with the diameter of about 2 mm; winding the carbon fiber rope on a die along threads according to a mechanical design manual, fixing three dies by using a graphite clamp, and fixing two ends of the carbon fiber rope;
step three: and (4) toughening the spring preform. And (3) putting the spring preform obtained in the step one into a deposition furnace, decomposing at 850 ℃ by adopting a chemical vapor infiltration method and taking propylene as a gas source, and preparing pyrolytic carbon (PyC) layers on the surface and inside of the preform, wherein the thickness of the pyrolytic carbon layers is about 200 nm.
Step four: and depositing the SiC substrate and the coating on the spring preform. And (3) putting the spring preform obtained in the step (2) into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as a carrier gas, argon as a diluent gas, and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 1000 ℃, 5kPa and 0.01MPa in the furnace, and depositing the SiC in the preform and on the surface of the preform to form a substrate and a coating.
Step five: and (6) demolding. Removing graphite clamps at two ends of the mold, drawing out the mold core, converging the external mold, drawing out the mold core from the interior of the spring to obtain the C/SiC composite material spring, wherein the density is 2.000 +/-0.05 g/cm measured according to an Archimedes drainage method3。
Example 4.
The spring has the mechanical parameters shown in the table 2, the rigidity of the spring at room temperature reaches 0.984N/mm, the rigidity of the spring in the air at 1000 ℃ still reaches 0.351N/mm, and the rigidity retention rate exceeds 35.6 percent.
The method comprises the following steps: preparation of spring forming die
According to a mechanical design manual, mechanical design parameters of the spring shown in the table 2 are designed, and a cylindrical ceramic mold which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing. The design concept of the die is mainly divided into two major aspects, on one hand, in order to ensure the smooth demoulding of the spring and the repeated utilization of the die, the die is divided into three parts along the axial direction, the dies on the two sides are provided with threads, through holes are distributed between the threads, the die in the middle part is longer than the other two parts for facilitating drawing and pulling, the side surface is not provided with the threads, and only the through holes distributed according to a spiral line are arranged; on the other hand, in order to ensure the stability of the mechanical parameters of the spring and the sufficiency of the deposition process, the whole die is designed into a hollow cylinder, threads are designed to fix carbon fibers, and through holes between the threads of the dies on two sides, on the side surface of the die in the middle and at the drawing part are designed.
Step two: and preparing a spring preform. 16 strands of carbon fibers (Dongli T300) are woven into a three-dimensional hollow tubular structure with the diameter of 2mm, and when the carbon fibers are wound on a die, the width of the carbon fibers perpendicular to the axial edge of the spring wire is 1.5 +/-0.5 mm, and the width of the carbon fibers parallel to the axial edge of the spring wire is 4.0 +/-0.5 mm. Winding the carbon fiber rope on a die along threads, fixing the three dies by using a graphite clamp, and fixing two ends of the carbon fiber rope;
step three: and (4) toughening the spring preform. And (3) putting the spring preform obtained in the step one into a deposition furnace, decomposing at 850 ℃ by adopting a chemical vapor infiltration method and taking propylene as a gas source, and preparing pyrolytic carbon (PyC) layers on the surface and inside of the preform, wherein the thickness of the pyrolytic carbon layers is about 200 nm.
Step four: and depositing the SiC substrate and the coating on the spring preform. And (3) putting the spring preform obtained in the step (2) into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as a carrier gas, argon as a diluent gas, and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 1000 ℃, 5kPa and 0.01MPa in the furnace, and depositing the SiC in the preform and on the surface of the preform to form a substrate and a coating.
Step five: and (6) demolding. Removing graphite clamps at two ends of the mold, drawing out the mold core, converging the outer mold, drawing out the mold core from the interior of the spring to obtain the C/SC composite material spring with the density of 2.000 +/-0.05 g/cm measured by an Archimedes drainage method3。
Example 5.
A spring made of a ceramic matrix composite according to the present invention as shown in FIG. 2(b) has a surface deposited with a coating layer, and the spring has a stiffness of 1.429N/mm at room temperature.
The method comprises the following steps: preparation of spring forming die
According to a mechanical design manual, mechanical design parameters of the spring shown in the table 1 are designed, and a cylindrical ceramic mold which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing. The design concept of the die is mainly divided into two major aspects, on one hand, in order to ensure the smooth demoulding of the spring and the repeated utilization of the die, the die is divided into three parts along the axial direction, the dies on the two sides are provided with threads, through holes are distributed between the threads, the die in the middle part is longer than the other two parts for facilitating drawing and pulling, the side surface is not provided with the threads, and only the through holes distributed according to a spiral line are arranged; on the other hand, in order to ensure the stability of the mechanical parameters of the spring and the sufficiency of the deposition process, the whole die is designed into a hollow cylinder, threads are designed to fix carbon fibers, and through holes between the threads of the dies on two sides, on the side surface of the die in the middle and at the drawing part are designed.
Step two: and preparing a spring preform. 16 strands of carbon fibers (Dongli T300) are woven into a three-dimensional hollow tubular structure with the diameter of 2mm, and when the carbon fibers are wound on a die, the width of the carbon fibers perpendicular to the axial edge of the spring wire is 1.5 +/-0.5 mm, and the width of the carbon fibers parallel to the axial edge of the spring wire is 4.0 +/-0.5 mm. And winding the carbon fiber rope on a die along the through hole, fixing the three dies by using a graphite clamp, and fixing two ends of the carbon fiber rope.
Step three: and (4) toughening the spring preform. And (3) putting the spring preform obtained in the step one into a deposition furnace, decomposing at 850 ℃ by adopting a chemical vapor infiltration method and taking propylene as a gas source, and preparing pyrolytic carbon (PyC) layers on the surface and inside of the preform, wherein the thickness of the pyrolytic carbon layers is about 200 nm.
Step four: and (5) forming and demolding the spring rough blank. And (3) placing the spring preform obtained in the step two into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as carrier gas, argon as diluent gas and trichloromethylsilane as a gas source, gradually decomposing the mixture into SiC under the conditions of 1000 ℃, 5kPa and 0.01MPa in the furnace, and depositing the SiC in the preform and on the surface of the preform to form a substrate and a coating.
Step five: and (6) demolding. Removing graphite clamps at two ends of the mold, drawing out the mold core, converging the external mold, drawing out the mold core from the interior of the spring to obtain the C/SiC composite material spring, wherein the density is 1.500 +/-0.050 g/cm measured according to an Archimedes drainage method3。
TABLE 1 mechanical parameters of elastic elements
TABLE 2 mechanical parameters of elastic elements
TABLE 3 Experimental parameters
Claims (4)
1. A preparation method of a continuous fiber reinforced C/SiC ceramic spring is characterized by comprising the following steps:
step 1, preparing a spring forming die: according to mechanical design parameters required by the spring, a cylindrical ceramic die which can be opened and closed, is provided with threads on the whole body and is provided with through holes distributed among the threads is obtained through three-dimensional software design and 3D printing; the die is hollow cylindrical and is divided into three sections along the axial direction, and the middle die is longer than the two end dies;
step 2, preparing a spring preform: fixing the three-section die by using a graphite clamp, weaving a plurality of strands of 1K, 3K or 12K carbon fibers into a carbon fiber rope, winding the carbon fiber rope on the die along threads on the whole body of the die, and fixing two ends of the carbon fiber rope to obtain a spring preform;
step 3, toughening the spring preform: placing the spring preform into a deposition furnace, decomposing the spring preform by adopting a chemical vapor infiltration method and taking propylene as an air source under the conditions of 850-1000 ℃ and 0.20-0.25 MPa of pressure in the furnace, and preparing pyrolytic carbon layers on the surface and inside of the preform;
step 4, depositing the SiC matrix and the coating on the spring preform: placing the spring preform processed in the step 3 into a deposition furnace, adopting a chemical vapor infiltration method, taking hydrogen as carrier gas, argon as diluent gas and trichloromethylsilane as a gas source, gradually decomposing the spring preform into SiC under the conditions of 950-1100 ℃ and the pressure in the furnace of 0.09-0.1 MPa, and depositing the SiC in the preform and on the surface of the preform to form a matrix and a coating;
step 5, demolding: and removing the graphite clamps at the two ends of the mold, drawing out the inner mold, converging the outer mold, and drawing out the outer mold from the spring to obtain the C/SiC composite material spring.
2. The method of manufacturing a continuous fiber reinforced C/SiC ceramic spring according to claim 1, characterized in that: the number of strands of the carbon fibers and the number of each strand are determined by the wire diameter of the spring wire required by the spring and the weaving method.
3. The method of manufacturing a continuous fiber reinforced C/SiC ceramic spring according to claim 1, characterized in that: the carbon fiber is woven into the carbon fiber rope by twisting the fibers or weaving the fibers in a mode of 1D, 2D or 3D.
4. The method of manufacturing a continuous fiber reinforced C/SiC ceramic spring according to claim 1, characterized in that: the pyrolytic carbon layer in the step 3 is a PyC or BN interface layer.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584307A (en) * | 2012-01-10 | 2012-07-18 | 中国人民解放军国防科学技术大学 | C/SiC ceramic matrix composite spring and preparation method thereof |
| CN102690124A (en) * | 2011-09-14 | 2012-09-26 | 中国人民解放军总后勤部军需装备研究所 | C/SiC ceramic matrix composite material and preparation method thereof |
| CN105016759A (en) * | 2015-07-01 | 2015-11-04 | 西北工业大学 | Rapid preparation method for C/SiC composite material |
| JP2018123023A (en) * | 2017-01-31 | 2018-08-09 | イビデン株式会社 | Method for producing ceramic spring, and the ceramic spring |
| CN109721377A (en) * | 2019-01-30 | 2019-05-07 | 湖南兴晟新材料科技有限公司 | Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof |
| CN109867527A (en) * | 2017-12-05 | 2019-06-11 | 辽宁法库陶瓷工程技术研究中心 | A kind of preparation method of photocuring 3D printing spiral type ceramics springs |
| CN110282981A (en) * | 2019-07-09 | 2019-09-27 | 西北工业大学 | Prepare the mold and method of the ceramic matric composite helical spring of SiC fiber |
-
2019
- 2019-11-21 CN CN201911145235.9A patent/CN110937909B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690124A (en) * | 2011-09-14 | 2012-09-26 | 中国人民解放军总后勤部军需装备研究所 | C/SiC ceramic matrix composite material and preparation method thereof |
| CN102584307A (en) * | 2012-01-10 | 2012-07-18 | 中国人民解放军国防科学技术大学 | C/SiC ceramic matrix composite spring and preparation method thereof |
| CN105016759A (en) * | 2015-07-01 | 2015-11-04 | 西北工业大学 | Rapid preparation method for C/SiC composite material |
| JP2018123023A (en) * | 2017-01-31 | 2018-08-09 | イビデン株式会社 | Method for producing ceramic spring, and the ceramic spring |
| CN109867527A (en) * | 2017-12-05 | 2019-06-11 | 辽宁法库陶瓷工程技术研究中心 | A kind of preparation method of photocuring 3D printing spiral type ceramics springs |
| CN109721377A (en) * | 2019-01-30 | 2019-05-07 | 湖南兴晟新材料科技有限公司 | Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof |
| CN110282981A (en) * | 2019-07-09 | 2019-09-27 | 西北工业大学 | Prepare the mold and method of the ceramic matric composite helical spring of SiC fiber |
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