CN114195546A - Heat-proof ring and preparation method thereof - Google Patents

Heat-proof ring and preparation method thereof Download PDF

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Publication number
CN114195546A
CN114195546A CN202111625441.7A CN202111625441A CN114195546A CN 114195546 A CN114195546 A CN 114195546A CN 202111625441 A CN202111625441 A CN 202111625441A CN 114195546 A CN114195546 A CN 114195546A
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heat
carbon fiber
fiber fabric
proof ring
silica sol
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邵长涛
韦其红
王洪升
刘小俊
朱保鑫
张萍萍
盖莹
翟萍
石江
苏通
高文秋
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Abstract

The invention discloses a preparation method of a heat-proof ring, which comprises the following steps: weaving carbon fiber fabric according to the shape and the size of the heat-proof ring; circularly compounding the carbon fiber fabric with first silica sol to obtain a prefabricated body; the preparation method comprises the following steps of carrying out hot pressing treatment on a prefabricated body to obtain the heat-proof ring, wherein the solid content of first silica sol is 23-50%, the volume fraction of carbon fiber fabrics in the heat-proof ring is 10-30%, and the heat-proof ring is further disclosed.

Description

Heat-proof ring and preparation method thereof
Technical Field
The invention belongs to the technical field of fiber-reinforced ceramic matrix composite materials, and particularly relates to a heat-proof ring and a preparation method thereof.
Background
The rudder wing and the cabin section of the weapon equipment are generally connected by metal alloy, along with the development of the weapon equipment to high Mach number and long endurance, the surface temperature of the connecting part of the rudder wing and the cabin section is higher and higher, in order to ensure the use reliability of the metal alloy connecting part, the connecting part needs to be thermally protected, the requirements of high temperature resistance, low heat conduction, ablation resistance and good thermal sealing performance and mechanical performance are provided for the heat-proof ring component, and the heat-proof ring component can rotate according to a certain angle when being used at high temperature.
The carbon fiber reinforced quartz ceramic matrix composite has the characteristics of small density, low heat conduction, high temperature resistance, fatigue resistance, creep resistance and small linear expansion coefficient, is a successful ablation material, is widely applied to the field of heat-proof materials, and in the prior art, for a heat-proof ring assembly with a complex shape and structure, a carbon fiber reinforced quartz ceramic matrix composite blank with a flat plate structure is firstly prepared, and then the blank is processed into the heat-proof ring assembly with a specific structure, but the heat-proof ring assembly prepared by the method has the following defects: (1) the heat-proof ring component is prepared by a continuous carbon fiber three-dimensional fabric through a process of infiltration method, slip casting molding, gel casting molding, hot-pressing sintering and the like, and because the product has larger size and thicker thickness, the heat-proof ring component is easy to have the phenomenon of internal unevenness in the molding process, the final product has a low-density area and finally influences the heat-proof performance, the figure 1 is a CT scanning image of a heat-proof blank body with a flat plate structure in the prior art, and the internal uniformity and the consistency of the heat-proof blank body with the flat plate structure can be seen from the figure 1, wherein the shadow part in the figure is the low-density area; secondly, quartz crystallization phenomenon exists in the heat-proof blank body with a flat plate structure in the hot pressing process, so that the mechanical property of the heat-proof blank body is reduced; meanwhile, in the subsequent processing, the continuous long fiber is broken, and the mechanical property of the continuous long fiber is further reduced.
Therefore, a heat-proof ring with excellent mechanical property and heat-proof property is needed.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention discloses a preparation method of a heat-proof ring with excellent heat-proof performance and mechanical performance, which adopts the following technical scheme:
a preparation method of the heat-proof ring comprises the following steps:
weaving carbon fiber fabric according to the shape and the size of the heat-proof ring;
circularly compounding the carbon fiber fabric with first silica sol to obtain a prefabricated body;
carrying out hot-pressing treatment on the prefabricated body to obtain a heat-proof ring,
the solid content of the first silica sol is 23-50%, and the volume fraction of the carbon fiber fabric in the heat-proof ring is 10-30%.
Further, before the hot pressing treatment of the preform, the method further comprises the following steps:
carrying out vacuum heat treatment on the prefabricated body, removing the surface compact layer, and circularly compounding second silica sol;
wherein the solid content of the second silica sol is 20-30%.
Further, the compounding method comprises the following steps which are carried out in sequence: vacuum impregnation, high pressure treatment and drying.
Further, the density of the preform compounded with the first silica sol is 1.40-1.50 g/cm3, and the density of the preform compounded with the second silica sol is 1.50-1.60 g/cm 3;
and/or
The thickness of the surface compact layer is 3-9 mm.
Further, before the compounding step, the organic impregnating compound on the surface of the carbon fiber fabric is removed through high-temperature heat treatment.
Further, the temperature of the hot pressing treatment is 1100-1250 ℃, the pressure is 15-30 MPa, and the time is 10-20 min.
Further, the temperature of the vacuum heat treatment is 800-1000 ℃, and the time is 1-2 hours.
Further, the vacuum degree of vacuum impregnation is-0.092 to-0.1 MPa, and the time is 1 to 3 hours;
the pressure of the high-pressure treatment is 7-10 MPa, and the time is 10-16 h;
the drying temperature is 100-180 ℃, and the drying time is 14-24 hours.
Further, the weaving method comprises the following steps:
designing a profiling weaving tool according to the shape and the size of the heat-proof ring, and weaving the carbon fiber fabric by utilizing the profiling weaving tool and combining a needling weaving mode with a normal sewing mode.
The invention also discloses a heat-proof ring which is prepared by adopting any one of the preparation methods.
By adopting the technical scheme, the invention has the beneficial effects that:
in the prior art, silica sol can only be compounded into the carbon fiber fabric from the upper surface, the lower surface and the side surface of the carbon fiber fabric with a flat plate structure, and the silica sol can be compounded into the carbon fiber fabric from the upper surface, the lower surface, the inner diameter surface and the outer diameter surface of the annular carbon fiber fabric by weaving the carbon fiber fabric according to the shape and the size of the heat-proof ring, so that the uniformity and the consistency of an inner quartz matrix of the heat-proof ring are improved; according to the invention, by reducing the volume fraction of the carbon fiber fabric in the heat-proof ring, the proportion of the nano quartz matrix is correspondingly increased, the pressure during hot-pressing treatment can be reduced, and the property of high surface energy of the nano quartz is utilized, so that the temperature and time of hot-pressing treatment are reduced, the carbon fiber fabric compounded with silica sol can be quickly softened at a lower temperature, and can be quickly compressed and molded under a lower pressure condition to release pores, thereby avoiding the possibility of crystallization of the carbon fiber fabric compounded with silica sol under the long-time high-temperature and high-pressure hot-pressing treatment condition, and improving the mechanical property of the heat-proof ring.
According to the invention, the prefabricated body is subjected to vacuum heat treatment, so that dried silica sol in the prefabricated body can shrink to generate shrinkage pores, the silica particles blocked on the surface of the prefabricated body during compounding can be removed by removing the surface compact layer, so that the shrinkage pores are exposed, and then the silica sol is continuously compounded in the shrinkage pores, so that the content of a quartz matrix in the prefabricated body is increased, and the compactness, uniformity and consistency in the heat-proof ring are improved.
Drawings
Fig. 1 is CT scanning pictures of different cross sections of a flat-plate structure heat-proof blank in the prior art.
FIG. 2 is a schematic view of a heat shield ring according to an embodiment of the present invention.
FIG. 3 is a thermal ring CT scan image according to an embodiment of the present invention.
Fig. 4 is a CT scan image of different cross-sections of the heat shield ring of fig. 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to solve the problems that the heat-proof ring component in the prior art is uniform in interior, poor in consistency, and prone to crystallization, and further influences the heat-proof effect of the heat-proof ring, the invention provides the heat-proof ring which is uniform in interior, free of crystallization, and good in heat-proof performance, and the preparation method of the heat-proof ring comprises the following steps:
weaving carbon fiber fabric according to the shape and the size of the heat-proof ring;
circularly compounding the carbon fiber fabric with first silica sol to obtain a prefabricated body;
carrying out hot-pressing treatment on the prefabricated body to obtain a heat-proof ring,
the solid content of the first silica sol is 23-50%, and the volume fraction of the carbon fiber fabric in the heat-proof ring is 10-30%.
Weaving a carbon fiber fabric according to the shape and the size of the heat-proof ring, and then circularly compounding the carbon fiber fabric and the first silica sol to obtain a prefabricated body, wherein the circular compounding refers to compounding the carbon fiber fabric and the first silica sol once, regulating the solid content of the first silica sol according to the density after the first compounding, compounding again, detecting the density after compounding, compounding again if the density does not meet the requirement until the density after compounding meets the requirement to obtain the prefabricated body, the solid content of the first silica sol is generally gradually reduced in the compounding process, and the density after compounding can generally reach 1.40-1.50 g/cm3Can be 1.40 to 1.50g/cm3As a density standard for the preform. And performing hot pressing treatment on the prefabricated body, wherein the hot pressing treatment mainly comprises softening the prefabricated body at high temperature, then compressing the prefabricated body at high pressure to release internal air holes, and performing finish machining according to the drawing requirements after the hot pressing treatment to obtain the heat-proof ring with better consistency, uniformity and mechanical property.
The heat-proof rings in the prior art are all prepared by preparing heat-proof materials with flat plate structures, then processing the heat-proof materials into the heat-proof rings according to the shapes and the sizes of the heat-proof rings, wherein the heat-proof rings are mainly applied to the metal alloy connecting parts of the rudder wings and the cabin sections of weapons, the sizes of the heat-proof materials are larger, the sizes of the heat-proof materials for processing the heat-proof rings are larger, the heat-proof materials with the large sizes of the flat plate structures are difficult to compound uniformly when being compounded with a quartz matrix, the common compounding mode is mainly impregnation, for example, the impregnation is adopted, the heat-proof materials with the flat plate structures can only be immersed from the upper surface, the lower surface and the side surfaces, the uniform immersion is difficult in the large-size flat plate structures, see figure 1, part a and part b in figure 1 are CT scanning pictures of different sections of heat-proof blanks with the flat plate structures, figure 1 shows that a large-area low-density area exists in the middle part of the flat plate structures, and the heat-proof rings processed by the flat plate structures, the internal uniformity and the consistency are also poor.
According to the invention, a traditional flat plate type weaving mode is abandoned, a profiling weaving scheme is adopted, the carbon fiber fabric is woven according to the shape and the size of the heat-proof ring, a structural schematic diagram of the heat-proof ring is shown in figure 2, and silica sol can be compounded into the carbon fiber fabric from the upper surface, the lower surface and the inner and outer diameter surfaces of the annular carbon fiber fabric during compounding, so that the uniformity and the consistency of the quartz matrix in the heat-proof ring are improved;
meanwhile, the whole inner cavity needs to be hollowed out when the flat-plate type heat-proof material is processed, continuous fibers can be broken at the moment, the reliability of the carbon fiber fabric as the support body is affected, the shape of the copying carbon fiber fabric does not need to be processed due to copying design, the continuous fibers do not need to be broken, and the reliability of the carbon fiber fabric as the support body is facilitated.
In the heat-proof material with a flat plate structure in the prior art, the volume fraction of the carbon fiber fabric is 30-40%, the volume fraction of the carbon fiber fabric is reduced to 10-30%, the proportion of a nano quartz matrix is correspondingly increased, the pressure during hot-pressing treatment can be reduced due to the increase of the amount of the nano powder, the temperature and time of hot-pressing treatment are reduced by utilizing the property of high surface energy of nano quartz, and when the prefabricated body is subjected to hot-pressing treatment, the carbon fiber fabric compounded with silica sol can be quickly softened at a lower temperature and quickly compressed and formed under a lower pressure condition to release air holes, so that the possibility that the carbon fiber fabric compounded with silica sol separates out quartz crystals under the condition of long-time high-temperature and high-pressure hot-pressing treatment is avoided, and the mechanical property of the heat-proof ring is improved.
According to the heat-proof material with the existing flat plate structure, the hot-pressing treatment temperature is 1300-1400 ℃, the pressure is 30-50 Mpa, and the time is 40-60 min, the hot-pressing treatment temperature can be reduced to 1100-1250 ℃, the pressure can be reduced to 15-30 Mpa, and the time can be shortened to 10-20 min by adjusting the proportion of the carbon fiber fabric and the quartz matrix in the heat-proof ring, so that the crystallization phenomenon of the quartz matrix is inhibited to a certain extent, and meanwhile, the compression amount of the hot-pressing treatment is about 20-40%.
Although the internal uniformity, consistency and mechanical property of the heat-proof ring prepared by the method are superior to those of the existing heat-proof material with a flat plate structure, when silica sol is compounded, silica particles are easily adsorbed on the surface of a prefabricated body, so that the pore diameter of the surface is blocked, the adsorption of the silica sol in the prefabricated body is influenced, meanwhile, the silica sol can shrink in a certain volume at high temperature, so that the inside of a blank material has great nonuniformity and inconsistency, and if the silica sol is directly subjected to hot pressing, the problems of the internal uniformity, consistency and the like of the heat-proof ring after hot pressing still exist.
In order to solve the problems, the method also comprises the following steps before the hot pressing treatment of the prefabricated body:
and carrying out vacuum heat treatment on the prefabricated body, removing the surface compact layer, and circularly compounding second silica sol, wherein the solid content of the second silica sol can be 20-30%, the temperature of the vacuum heat treatment can be 800-1000 ℃, and the time is 10-30 min.
According to the invention, the prefabricated body is subjected to vacuum treatment, so that dried silica sol in the prefabricated body shrinks to generate shrinkage pores, then the surface compact layer on the surface of the prefabricated body is removed, namely silica particles blocked on the surface of the prefabricated body during compounding are removed, the shrinkage pores can be exposed, and the silica sol is compounded in the shrinkage pores in a circulating manner again, so that the density of a quartz matrix in the prefabricated body can be improved, the interlayer bonding strength of the finally prepared heat-proof ring is improved, and after the second silica sol is compounded, the density of the prefabricated body can be generally improved to 1.50-1.60 g/cm3Can be 1.50 to 1.60g/cm3As the density standard of the preform after the second cycle compounding.
After twice circulating compounding, the uniformity and consistency inside the blank material are better, when hot pressing treatment is carried out, the inside of the hot-pressed heat release ring is more compact and uniform, and the density of the finally prepared heat-proof ring can reach 2.05g/cm3The above.
The thickness of the surface compact layer is generally 3-9 mm, because a preform prepared by profiling generally has a machining allowance of 5-10 mm relative to a heat-proof ring, shrinkage pores in the preform can be opened by removing the surface compact layer, on the other hand, the preform is reduced, the machining allowance is controlled, subsequent finish machining is facilitated, the machining allowance is generally controlled to be 1-2 mm, therefore, the thickness of the surface compact layer which is preferably removed is 3-9 mm, and the specific amount can be adjusted according to the actual machining size.
Furthermore, for better profile knitting, the profile knitting tool can be designed according to the shape and the size of a finished product of the heatproof ring, the profile knitting tool can be made of plastic or metal, the knitting method can be a mode of combining a needle punching knitting mode with normal sewing, the sewing distance of the normal sewing is 5 +/-1 mm, and long fibers are adopted for the normal sewing, so that the interlaminar shearing performance of the carbon fiber fabric can be improved.
The density of the heat-proof ring is required to be more than or equal to 2.0g/cm to achieve the qualified heat-proof performance3The interlaminar shear strength is more than or equal to 15MPa, and the compressive strength is more than or equal to 170 MPa. The carbon fiber fabric is woven by adopting a commonly-used 2.5D structure and an orthogonal three-dimensional structure, and the density of the final material is more than or equal to 1.90g/cm3The compression strength is more than 120MPa, and the volume fraction of the carbon fiber fabric is more than 30 percent, which can not meet the requirements, the invention adopts the needling structure to weave the carbon fiber fabric, the needling structure carbon fiber fabric can ensure the comprehensive performance of the composite material through the design of the proportion of long fibers and short fibers of the fabric, the warp-weft density and the surface density of the carbon fiber fabric, and the like, the structure has the advantages that the performance in the plane direction has isotropy, and simultaneously, the uniformity and the consistency of the carbon fiber fabric prepared by the method are optimal.
The carbon fiber fabric is high in interlaminar shear strength due to the introduction of normal fibers, damage to continuous carbon fibers is reduced in the subsequent processing process due to the profiling weaving, and simultaneously, through twice circulating compounding, the content of a quartz matrix in the composite material is increased, and the temperature, pressure and time of hot-pressing sintering are reduced, so that even if the volume fraction of the carbon fiber fabric is reduced, the mechanical property of the heat-proof ring is not reduced, and on the contrary, the mechanical property of the heat-proof ring is further improved by controlling crystallization.
Furthermore, the carbon fiber fabric is formed by adopting a needling structure and profiling weaving and is an annular fabric with a certain wall thickness and height, and in the preparation process of the carbon fiber, in order to improve the weaving performance of the fiber, an organic impregnating compound coating needs to be made on the surface of the carbon fiber so as to be beneficial to weaving the carbon fiber; the presence of the organic impregnating compound on the surface of the fiber can cause the performance reduction of the subsequent composite material, so that the organic impregnating compound coating needs to be removed through high-temperature heat treatment before composite molding, and the conditions of the high-temperature heat treatment can be as follows: and treating the carbon fiber fabric for 1-2 hours at 900-1000 ℃ in a vacuum atmosphere.
In the high-temperature heat treatment process, in order to prevent the deformation of the carbon fiber fabric, a graphite or quartz ceramic raw material can be adopted, the size and the dimension of the heat-proof ring are simulated, a profiling positioning tool is prepared, the carbon fiber is clamped and positioned, and the deformation of the carbon fiber fabric in the high-temperature heat treatment process is avoided.
Further, the compounding process of the present invention comprises the following steps performed in sequence:
vacuum impregnation: the vacuum degree during vacuum impregnation can be-0.092 to-0.1 MPa, and the impregnation time can be 1 to 3 hours;
high-pressure treatment: the method can be carried out in high-pressure equipment such as a high-pressure reaction kettle and the like, the pressure is 7-10 Mpa, and the time for keeping the pressure is 10-16 h;
thirdly, drying: the method can be carried out in drying equipment such as a drying oven, and the drying temperature is 100-180 ℃, and the drying time is 14-24 hours.
Meanwhile, in order to prevent the carbon fiber fabric from deforming in the compounding process, a porous metal profiling compounding tool can be prepared according to the shape and size of the heat-proof ring, the carbon fiber fabric is clamped on the profiling compounding tool for compounding, and the compounding mode of compounding the first silica sol and the second silica sol can adopt the steps.
Several groups of specific examples of the invention for the preparation of the heat-protective ring will be disclosed below:
example 1
The method comprises the following steps: weaving the carbon fiber fabric by using a profiling weaving tool and adopting a needling structure and a normal sewing mode, wherein the volume fraction of the carbon fiber fabric is controlled to be 10%, and the normal sewing distance is 5 mm;
step two: clamping the carbon fiber fabric on a profiling positioning tool, and pretreating the carbon fiber fabric for 1h at 900 ℃ in a vacuum atmosphere;
step three: clamping the carbon fiber fabric on a profiling composite tool, and circularly compounding the first silica sol for multiple times until the density of the carbon fiber fabric compounded with the first silica sol reaches 1.40g/cm3So as to obtain the prefabricated body,
the compounding steps are specifically as follows: dipping for 1h in a vacuum environment of-0.092 MPa; keeping the pressure in a 7MPa high-pressure reaction kettle for 10 hours; drying in a drying oven at 100 deg.C 14.
Step four: placing the prefabricated body in a vacuum environment at 800 ℃ for heat treatment for 10min, then removing a surface compact layer with the thickness of 3mm, and continuously and circularly compounding the second silica sol until the density of the carbon fiber fabric compounded with the second silica sol reaches 1.50g/cm3The cyclic compounding method is the same as the third step;
step five: the density is up to 1.50g/cm3The prefabricated body is arranged in a hot-pressing die, the prefabricated body is guaranteed not to deform in the diameter direction, hot-pressing treatment is carried out, the temperature is 1100 ℃, the pressure is 15MPa, the time is 10min, and after the prefabricated body is taken out, the heat-proof ring is obtained through finish machining according to the drawing.
Example 2
The method comprises the following steps: weaving the carbon fiber fabric by using a profiling weaving tool and adopting a needling structure and a normal sewing mode, wherein the volume fraction of the carbon fiber fabric is controlled to be 30%, and the normal sewing distance is 6 mm;
step two: clamping the carbon fiber fabric on a profiling positioning tool, and pretreating the carbon fiber fabric for 2 hours at 1000 ℃ in a vacuum atmosphere;
step three: clamping the carbon fiber fabric on a profiling composite tool, and circularly compounding the first silica sol for multiple times until the density of the carbon fiber fabric compounded with the first silica sol reaches 1.50 g/bamboocm3So as to obtain the prefabricated body,
the compounding steps are specifically as follows: dipping for 3h under a vacuum environment of-0.1 MPa; keeping the pressure in a high-pressure reaction kettle with the pressure of 10MPa for 16 h; drying at 180 deg.C for 24 hr.
Step four: placing the prefabricated body in a vacuum environment at 1000 ℃ for heat treatment for 30min, then removing a surface compact layer with the thickness of 9mm, and continuously and circularly compounding the second silica sol until the density of the carbon fiber fabric compounded with the second silica sol reaches 1.60g/cm3The cyclic compounding method is the same as the third step;
step five: the density is up to 1.60g/cm3The prefabricated body is arranged in a hot-pressing die, the prefabricated body is guaranteed not to deform in the diameter direction, hot-pressing treatment is carried out, the temperature is 1250 ℃, the pressure is 30MPa, the time is 20min, and the prefabricated body is taken out and then is subjected to finish machining according to a drawing to obtain the heat-proof ring.
Example 3
The method comprises the following steps: weaving the carbon fiber fabric by using a profiling weaving tool and adopting a needling structure and a normal sewing mode, wherein the volume fraction of the carbon fiber fabric is controlled to be 20%, and the normal sewing distance is 4 mm;
step two: clamping the carbon fiber fabric on a profiling positioning tool, and pretreating the carbon fiber fabric for 1.5 hours at 950 ℃ in a vacuum atmosphere;
step three: clamping the carbon fiber fabric on a profiling composite tool, and circularly compounding the first silica sol for multiple times until the density of the carbon fiber fabric compounded with the first silica sol reaches 1.45g/cm3So as to obtain the prefabricated body,
the compounding steps are specifically as follows: dipping for 2h under a vacuum environment of-0.096 MPa; keeping the pressure in a high-pressure reaction kettle of 8MPa for 13 h; drying at 140 deg.C for 19 h.
Step four: placing the prefabricated body in a vacuum environment at 900 ℃ for heat treatment for 20min, then removing a surface compact layer with the thickness of 6mm, and continuously and circularly compounding the second silica sol until the density of the carbon fiber fabric compounded with the second silica sol reaches 1.55g/cm3The cyclic compounding method is the same as the third step;
step five: the density is up to 1.55g/cm3Is made of a preformAnd putting the prefabricated part into a hot-pressing die, ensuring that the prefabricated part does not deform in the diameter direction, carrying out hot-pressing treatment at the temperature of 1200 ℃, under the pressure of 20MPa for 15min, and taking out the prefabricated part and carrying out finish machining according to a drawing to obtain the heat-proof ring.
Fig. 3 is a CT scan of the heat protection ring obtained in example 3, and c, d, and e in fig. 4 are CT scans of different cross sections of the heat protection ring of example 3 (i.e., fig. 3), and it can be seen from fig. 4 that the heat protection ring prepared by the present invention has good uniformity and consistency, and uniform density at each position.
After the heat-proof rings in the embodiment 3 are assembled, high-temperature air tightness performance examination is carried out, and the air tightness performance meets the requirements under the required high-temperature examination conditions; the rudder shaft can rotate in the test process, the application requirement can be met, and the detected density of the heat-proof ring is more than or equal to 2.05g/cm3The interlaminar shear strength is not less than 19MPa, the compression strength is not less than 170MPa, and the heat-proof performance is better.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still modify the technical solutions described in the foregoing embodiments, or may equally substitute some or all of the technical features; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.

Claims (10)

1. A preparation method of a heat-proof ring is characterized by comprising the following steps: the method comprises the following steps:
weaving carbon fiber fabric according to the shape and the size of the heat-proof ring;
circularly compounding the carbon fiber fabric with first silica sol to obtain a prefabricated body;
carrying out hot-pressing treatment on the prefabricated body to obtain a heat-proof ring,
the solid content of the first silica sol is 23-50%, and the volume fraction of the carbon fiber fabric in the heat-proof ring is 10-30%.
2. The method of claim 1, wherein: before the prefabricated body is subjected to hot pressing treatment, the method also comprises the following steps:
carrying out vacuum heat treatment on the prefabricated body, removing the surface compact layer, and circularly compounding second silica sol;
wherein the solid content of the second silica sol is 20-30%.
3. The production method according to claim 1 or 2, characterized in that:
the compounding method comprises the following steps of: vacuum impregnation, high pressure treatment and drying.
4. The method of claim 2, wherein:
the density of the preform compounded with the first silica sol is 1.40-1.50 g/cm3The density of the preform compounded with the second silica sol is 1.50-1.60 g/cm3
And/or
The thickness of the surface compact layer is 3-9 mm.
5. The method of claim 1, wherein: before the compounding step, the organic impregnating compound on the surface of the carbon fiber fabric is removed through high-temperature heat treatment.
6. The method of claim 1, wherein:
the hot-pressing treatment temperature is 1100-1250 ℃, the pressure is 15-30 MPa, and the time is 10-20 min.
7. The method of claim 2, wherein:
the temperature of the vacuum heat treatment is 800-1000 ℃, and the time is 1-2 h.
8. The production method according to claim 3, characterized in that:
the vacuum degree of the vacuum impregnation is-0.092 to-0.1 MPa, and the time is 1 to 3 hours;
the pressure of the high-pressure treatment is 7-10 MPa, and the time is 10-16 h;
the drying temperature is 100-180 ℃, and the drying time is 14-24 hours.
9. The method of claim 1, wherein: the weaving method comprises the following steps:
designing a profiling weaving tool according to the shape and the size of the heat-proof ring, and weaving the carbon fiber fabric by utilizing the profiling weaving tool and combining a needling weaving mode with a normal sewing mode.
10. A heat shroud, characterized by: the preparation method of any one of claims 1 to 9.
CN202111625441.7A 2021-12-28 2021-12-28 Heat-proof ring and preparation method thereof Pending CN114195546A (en)

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