CN118580090B - A preparation method of quartz composite material and quartz composite material - Google Patents
A preparation method of quartz composite material and quartz composite material Download PDFInfo
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- CN118580090B CN118580090B CN202411065688.1A CN202411065688A CN118580090B CN 118580090 B CN118580090 B CN 118580090B CN 202411065688 A CN202411065688 A CN 202411065688A CN 118580090 B CN118580090 B CN 118580090B
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Abstract
The application provides a preparation method of a quartz composite material and the quartz composite material, wherein the preparation method of the quartz composite material mainly comprises the steps of manufacturing a first prefabricated braided fabric, preprocessing the first prefabricated braided fabric, carrying out high-temperature aerobic processing and carrying out at least three times of dipping processing on the first prefabricated braided fabric by utilizing acidic silica sol, so as to obtain a prefabricated body, then placing the prefabricated body in a high-temperature furnace at 700-800 ℃ for 3-4 h, then cooling the high-temperature furnace to room temperature, and then taking out the prefabricated body, thus obtaining the quartz composite material. The quartz composite material prepared by the preparation method of the quartz composite material can realize the tight combination of the titanium alloy wire and the quartz fiber, lay a foundation for the later welding process of the quartz composite material and metal parts, further realize the tight connection with other metal parts, and meet the performance requirements of mechanics, thermal and the like under special working conditions.
Description
Technical Field
The application relates to the technical field of composite materials, in particular to a preparation method of a quartz composite material and the quartz composite material.
Background
The multifunctional composite material is a current research hotspot, and has wide application prospects in the fields of aerospace, missile, transportation and the like, wherein in the field of missile, the radome is an important part of the missile, is positioned at the head of an aircraft, and is a part integrating wave transmission, heat prevention, bearing, corrosion resistance and the like. Therefore, the materials applied to the radome generally need to have at least three functions of heat prevention, wave transmission and bearing, in addition, the quartz composite radome positioned at the head of the aircraft needs to be tightly connected with a missile metal elastomer or other material parts in a certain connection mode and bear the performance requirements of mechanics, heat and the like under the working state of the missile, so that the corresponding functions of the missile can be realized. The welding process is a novel process for realizing the connection of the ceramic material and the metal material. For the quartz composite material and the titanium alloy material, because of the large expansion coefficient difference, the firm connection of the two materials is difficult to realize by a direct welding method.
There is therefore a need for a new composite material that overcomes the above technical problems.
Disclosure of Invention
In order to overcome the technical problems in the prior art, the application provides a preparation method of a quartz composite material and the quartz composite material, so that the quartz composite material provided by the application has good connection performance, and further the problems in the background art can be solved.
The application provides a preparation method of a quartz composite material, which comprises the following steps:
Step S1: mixing quartz fiber cloth and metal wires in a layering manner to obtain a mixed piece, and then using fiber yarns to manufacture the mixed piece into a first prefabricated braided fabric in a sewing manner, wherein the first prefabricated braided fabric is in a flat plate shape, a rotary body cone shape or a special-shaped structure shape, and sequentially treating the first prefabricated braided fabric in the following manner to obtain a prefabricated body;
Step S2: placing the first prefabricated braided fabric in a high-temperature furnace, heating the high-temperature furnace to 450-500 ℃ and maintaining the temperature for 2-4 hours, so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition;
step S3: taking the first prefabricated braided fabric out of the high-temperature furnace, placing the first prefabricated braided fabric into an impregnating tank, and carrying out impregnation treatment on the first prefabricated braided fabric by using first acidic silica sol;
Step S4: placing the dipping tank in an oven, setting the temperature of the oven at 40-60 ℃ and maintaining until the first acidic silica sol is completely changed into a solid state;
step S5: taking the first prefabricated braided fabric out of the dipping tank and placing the first prefabricated braided fabric in the high-temperature furnace, and heating the high-temperature furnace to 400-500 ℃ so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition;
Step S6: taking the first prefabricated braided fabric out of the high-temperature furnace, placing the first prefabricated braided fabric into an impregnating tank, and carrying out impregnation treatment on the first prefabricated braided fabric by using second acidic silica sol;
step S7: placing the first prefabricated braided fabric in an oven, setting the temperature of the oven to be 70-100 ℃, and keeping the first prefabricated braided fabric at 70-100 ℃ for 2-4 hours; transferring the first prefabricated braided fabric into the high temperature furnace, heating the high temperature furnace to 400-500 ℃ and maintaining the temperature for 2-4 hours, so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high temperature condition;
step S8: repeating the step S6 and the step S7 at least twice to obtain the prefabricated body;
step S9: and taking out the preform, placing the preform in the high-temperature furnace, controlling the high-temperature furnace to heat to 700-800 ℃ at 2-4 ℃/min, placing the preform for 3-4 h, then cooling the high-temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
In some embodiments, a pumping pipeline is arranged on the dipping tank and is used for sucking the first acidic silica sol or the second acidic silica sol into the dipping tank;
in addition, the step S3 further includes the following steps:
step S31: pumping air from the interior of the dipping tank through a vacuum pump so as to enable the interior of the dipping tank to be in a negative pressure state, and keeping the negative pressure state for 10-20 min;
Step S32: sucking the first acidic silica sol into the impregnation tank through the material sucking pipeline, immersing the first prefabricated braided fabric in the first acidic silica sol, and keeping the negative pressure state in the impregnation tank unchanged all the time in the process of sucking the first acidic silica sol;
step S33: closing the pumping pipeline, and continuously maintaining the vacuum pump to continuously pump the impregnating tank so as to maintain the impregnating tank in a negative pressure state for 60-120 min;
step S34: and closing the vacuum pump to restore the inside of the dipping tank to a normal pressure state.
In some embodiments, the wires are laid in a manner that the distance is 2 mm-4mm to form a wire mesh;
and the layering mode is to lay a layer of the wire mesh between every two layers of quartz fiber cloth so as to form the mixing piece.
In some embodiments, the material of the metal wire may be any one of TC4 titanium alloy wire and TC6 titanium alloy wire;
the fiber yarn has a tex value of any one of 570, 190 and 195.
In some embodiments, the diameter of the wire is phi 0.05mm to 0.1mm;
The sewing mode is a lock type penetrating sewing process or a temporary sewing process, and the sewing needle distance of the sewing mode is 4 mm-5 mm.
In some embodiments, the quartz fiber cloth may be a quartz glass fiber satin cloth with a thickness of 0.1mm to 0.3 mm.
In some embodiments, the first acidic silica sol concentration is 45% -50%;
the concentration of the second acidic silica sol is 25% -40%.
In some embodiments, the negative pressure state has a pressure of negative 0.095mpa to 0.1mpa.
In some embodiments, the first preform braid is flat, gyrorotor cone-shaped, or shaped in a contoured configuration.
In some embodiments, the application also provides a quartz composite material prepared by the method for preparing the quartz composite material in any of the embodiments.
The invention has at least the following beneficial effects:
1. The preparation method of the quartz composite material provided by the invention realizes the preparation and engineering application of the high-strength and high-efficiency heat-insulation composite material by mixing and braiding quartz and metal, and then carrying out high-temperature oxidation and repeated impregnation processes, and has excellent application prospect;
2. The quartz composite material prepared by the preparation method provided by the invention can realize the tight combination of the titanium alloy wire and the quartz fiber, lay a foundation for the later welding process of the quartz composite material and metal parts, realize the tight connection with other metal parts, and meet the performance requirements of mechanics, heat and the like in a special working state, thereby being applicable to the field of missiles;
3. The quartz composite material prepared by the preparation method provided by the invention can be suitable for a first prefabricated braided fabric with a specific shape, such as a flat plate shape, a conical rotation shape or an ellipsoidal shape, thereby being beneficial to realizing the welding connection molding of the quartz composite material and a metal part and expanding the application range of the quartz composite material.
Detailed Description
Further advantages and effects of the present application will become apparent to those skilled in the art from the disclosure of the present specification, by describing the embodiments of the present application with specific examples. While the description of the application will be presented in connection with certain embodiments, it is not intended to limit the features of this application to only this embodiment. Rather, the purpose of the present application is to cover other alternatives or modifications, which may be extended by the claims based on the application. The following description contains many specific details for the purpose of providing a thorough understanding of the present application. The application may be practiced without these specific details. Furthermore, some specific details are omitted from the description in order to avoid obscuring the application. It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other.
The embodiment of the application provides a preparation method of a quartz composite material, which comprises the following steps: step S1: mixing quartz fiber cloth and metal wires in a layering mode to obtain a mixed piece, manufacturing the mixed piece into a first prefabricated braided fabric by utilizing fiber yarns in a sewing mode, sequentially processing the first prefabricated braided fabric in the following mode to obtain a prefabricated body, and step S2: placing the first prefabricated braided fabric in a high-temperature furnace, heating the high-temperature furnace to 450-500 ℃ and maintaining the temperature for 2-4 hours, so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition; step S3: taking the first prefabricated braided fabric out of the high-temperature furnace, placing the first prefabricated braided fabric in an impregnating tank, and carrying out impregnation treatment on the first prefabricated braided fabric by using first acidic silica sol; step S4: placing the dipping tank in an oven, setting the temperature of the oven at 40-60 ℃ and maintaining until the first acidic silica sol is completely changed into a solid state; step S5: taking out the first prefabricated braided fabric from the impregnation tank, placing the first prefabricated braided fabric in a high-temperature furnace, and heating the high-temperature furnace to 400-500 ℃ so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition; step S6: taking the first prefabricated braided fabric out of the high-temperature furnace, placing the first prefabricated braided fabric in an impregnating tank, and carrying out impregnation treatment on the first prefabricated braided fabric by using second acidic silica sol; step S7: placing the first prefabricated braided fabric in an oven, setting the temperature of the oven to be 70-100 ℃, and keeping the first prefabricated braided fabric at the temperature of 70-100 ℃ for 2-4 hours; transferring the first prefabricated braided fabric into a high-temperature furnace, heating the high-temperature furnace to 400-500 ℃ and maintaining the temperature for 2-4 hours, so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition; step S8: repeating the step S6 and the step S7 at least twice to obtain the prefabricated body; step S9: taking out the preform, placing the preform in a high temperature furnace, controlling the high temperature furnace to heat to 700-800 ℃ at 2-4 ℃/min, placing the preform for 3-4 h, then cooling the high temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
Specifically, quartz fiber cloth mixes with the wire with the layering mode, and then can intensive mixing fully contact, and the reuse fiber yarn is woven the hybrid to make the mixture can remain mixed state throughout in a series of follow-up dipping and high temperature treatment, in order to avoid the material to scatter, and then lead to the condition emergence that the final product performance of material is not good. And then, the first prefabricated braided fabric is softened by high-temperature aerobic treatment so as to be further mixed and combined, and then, the impregnation treatment is carried out by using acidic silica sol.
In some embodiments, the impregnating tank is provided with a pumping pipeline for sucking the first acidic silica sol or the second acidic silica sol into the impregnating tank; in addition, the step S3 further includes the following steps: step S31: pumping air from the interior of the dipping tank through a vacuum pump to enable the interior of the dipping tank to be in a negative pressure state, and keeping the negative pressure state for 10-20 min; step S32: sucking the first acidic silica sol into the impregnating tank through a material sucking pipeline, immersing the first prefabricated braided fabric in the first acidic silica sol, and keeping the negative pressure state in the impregnating tank unchanged all the time in the process of sucking the first acidic silica sol; step S33: closing the material pumping pipeline, and continuously maintaining the vacuum pump to continuously pump air out of the dipping tank so as to maintain the dipping tank in a negative pressure state for 60-120 min; step S34: the vacuum pump is turned off to restore the inside of the dipping tank to a normal pressure state.
In particular, the negative pressure environment helps to penetrate the silicic acid gum solution into the micropores of the substrate more rapidly. By applying negative pressure, the gas in the porous material can be discharged, so that a negative pressure state is formed in the impregnating tank, and the impregnating liquid can rapidly fill the gaps of the material.
Due to the negative pressure effect, capillary force in the impregnation process is enhanced, so that the impregnation speed is increased, the material can be further embedded into the internal structure, and a more uniform and thorough impregnation effect is realized, so that the contact between the first acidic silica sol or the second acidic silica sol and the surface of the carrier is promoted, intermolecular interaction force is enhanced, durability and stability of a final product are improved, time required by the impregnation process is effectively reduced, production efficiency is improved, the penetration depth and uniformity of the impregnation liquid to the material are adjusted, and therefore, various physical and chemical properties of the material are optimized.
In some embodiments, the wires are laid in a manner that the spacing is 2 mm-4 mm to form a wire mesh, and the layering manner is to lay a layer of wire mesh between every two layers of quartz fiber cloth to form a hybrid.
Specifically, through experiments for many times, when the interval of the metal wires in the metal wire mesh is 2mm ~4mm for in guaranteeing the compact structure of first prefabricated knitting, can make first acid silica sol or second acid silica sol fully permeate in the hole, and then can go deep into the inner structure of first prefabricated knitting more, realize more even and thorough flooding effect, thereby effectively ensured the comprehensive properties of end product, the setting of spreading one deck metal wire mesh between two-layer quartz fiber cloth in addition, make the mixed effect between quartz fiber cloth and the metal wire mesh better, and then provide the guarantee for the comprehensive properties of end product.
In some embodiments, the metal wire may be any one of TC4 titanium alloy wire and TC6 titanium alloy wire, and the fiber yarn has a tex value of any one of 570, 190, and 195.
Specifically, the TC4 titanium alloy wire has excellent specific strength and corrosion resistance and good weldability, the TC4 titanium alloy wire is doped in the quartz composite material so as to effectively improve the welding performance of the quartz composite material, in addition, fiber yarns with different thicknesses can be selected according to actual requirements, and a plurality of experimental results show that the fiber yarns with high requirements on durability and cost can be adopted, the fiber yarns with high requirements on tensile property and air permeability can be adopted, and the fiber yarns with high requirements on elastic property and comprehensive performance can be adopted, and the fiber yarns with the tex value of 195 can be adopted.
In some embodiments, the wire has a diameter of from 0.05mm to 0.1mm, the stitching is a lock-through stitching process or a face stitching process, and the stitch gauge of the stitching is from 4mm to 5mm.
In particular, experiments show that when the diameter of the metal wire is phi 0.05 mm-0.1 mm, the mixture can react more fully under the high temperature condition and in the dipping treatment process, so that the final product can obtain better performance, in addition, the bonding force between quartz composite material layers can be increased by sewing fibers in the thickness direction by adopting a locking type penetrating sewing process, layering phenomenon is effectively prevented, and further interlayer strength is improved, meanwhile, by increasing bonding force between layers, dispersion and absorption of impact energy are facilitated, and further impact resistance is enhanced, by connecting each ply, hollows and gaps inside the material are reduced, the structural integrity of the composite material is improved, the effect of optimizing the structural integrity is achieved, and further, the performances such as stretching, compression and the like of the quartz composite material can be remarkably improved according to the specific sewing mode and parameter adjustment.
It should be noted that the stitching process can also be adopted to stitch, and the effect of improving the stretching, compression and bending properties of the quartz composite material can be achieved.
In some embodiments, the quartz fiber cloth may be a satin cloth of quartz glass fibers having a thickness of 0.1mm to 0.3 mm.
Specifically, the quartz glass fiber satin is a special glass fiber fabric with high performance, and can provide a high-quality performance foundation for the quartz composite material.
In some embodiments, the first acidic silica sol concentration is 45% -50%; the concentration of the second acidic silica sol is 25% -40%.
In some embodiments, the negative pressure state is at a negative pressure of 0.095mpa to 0.1mpa.
Specifically, the experimental results show that when the negative pressure is in the negative pressure range of 0.095-0.1 mpa, the acidic silica sol can better penetrate into the material, and the excellent performance of the material is not affected.
In some embodiments, the first preformed braid is flat, gyrorotor cone-shaped, or shaped.
The application also provides a quartz composite material, which is prepared by the preparation method of the quartz composite material in any embodiment.
Specifically, the quartz composite material prepared by the preparation method provided by the application has excellent comprehensive performance.
The invention will be further illustrated by way of example, but the scope of the invention is not limited to these examples.
Example 1
And preparing the tabular quartz composite material according to the target shape and the target size of the quartz composite material.
The preparation method of the quartz composite material comprises the following steps:
step S1: making a first prefabricated braided fabric: mixing quartz fiber cloth and metal wires in a layering mode, preparing a first prefabricated braided fabric with a flat plate structure by adopting a quartz fiber yarn puncture sewing process, and sequentially processing the first prefabricated braided fabric by adopting the following modes to prepare a prefabricated body; wherein, the technological parameters of the sewing mode are shown in the following table 1;
Step S2: performing a first pre-made braid pretreatment: placing the first prefabricated braided fabric in a high-temperature furnace, and heating the high-temperature furnace to 475 ℃ so that the first prefabricated braided fabric is treated for 3 hours in a high-temperature aerobic environment;
step S3: dipping treatment: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnation tank, sealing a tank cover of the impregnation tank, pumping air to the inside of the impregnation tank to negative pressure of 0.1Mpa by a vacuum pump, and keeping the negative pressure condition for 10min; sucking the acidic silica sol with the concentration value of 50% into the impregnation tank through a material sucking pipeline preset on the impregnation tank by utilizing the negative pressure environment in the impregnation tank, immersing the acidic silica sol into the first prefabricated braided fabric, and keeping the negative pressure state in the impregnation tank unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining the vacuum pump to pump air to the dipping tank, maintaining the pressure of the dipping tank in a negative pressure state at negative 0.1Mpa for 120min, closing the vacuum pump, and recovering the dipping tank to a normal pressure state; opening a cover body of the dipping tank, placing the dipping tank in an oven, setting the temperature in the oven to be 50 ℃ and maintaining until the acidic silica sol is completely changed into a solid state;
step S4: taking out the first prefabricated braided fabric after the dipping treatment from the dipping tank, firstly removing attachments on the surface of the first prefabricated braided fabric, then placing the treated first prefabricated braided fabric in a high-temperature furnace, heating to 450 ℃, and treating for 3 hours under the aerobic condition;
step S5: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnating tank, pumping air from the impregnating tank through a vacuum pump until the inside of the impregnating tank is pumped, so that the inside of the impregnating tank is in a negative pressure state, the pressure of the negative pressure state is negative 0.1Mpa, and keeping the negative pressure state for 10min; the acidic silica sol with the concentration value of 30% can be sucked into the dipping tank through a preset pumping pipeline on the dipping tank by utilizing the negative pressure state in the dipping tank until the acidic silica sol submerges the first prefabricated braided fabric, and the negative pressure state in the dipping tank is kept unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining a vacuum pump to pump air from the dipping tank, maintaining the negative pressure state of 0.1Mpa of negative pressure in the dipping tank, closing the vacuum pump after 60min, and recovering the inside of the dipping tank to a normal pressure state; opening the cover body of the dipping tank, and taking out the first prefabricated braided fabric;
Step S6: placing the treated first prefabricated braided fabric into an oven, setting the temperature of the oven to 80 ℃, and maintaining the environment at 80 ℃ for 3 hours; transferring the first prefabricated braided fabric into a high-temperature furnace, heating to 450 ℃, and continuously treating for 3 hours under the aerobic condition;
step S7: sequentially repeating the step S5 and the step S6 twice to obtain a prefabricated body;
Step S8: taking out the preform, cleaning attachments on the surface of the preform, controlling a high-temperature furnace to heat to 800 ℃ at 2 ℃/min, placing the preform in an environment of 800 ℃ for 3 hours, then cooling the high-temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
Example 2
And preparing the tabular quartz composite material according to the target shape and the target size of the quartz composite material.
The preparation method of the quartz composite material comprises the following steps:
Step S1: making a first prefabricated braided fabric: mixing quartz fiber cloth and metal wires in a layering mode, preparing a first prefabricated braided fabric with a flat plate structure by adopting a quartz fiber yarn puncture sewing process, and sequentially processing the first prefabricated braided fabric by adopting the following modes to prepare a prefabricated body; wherein, the technological parameters of the sewing mode are shown in the following table 2;
Step S2: performing a first pre-made braid pretreatment: placing the first prefabricated braided fabric in a high-temperature furnace, and heating the high-temperature furnace to 490 ℃ to enable the first prefabricated braided fabric to be treated for 3 hours in a high-temperature aerobic environment;
Step S3: dipping treatment: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnation tank, sealing a tank cover of the impregnation tank, pumping air to the inside of the impregnation tank to negative pressure of 0.098Mpa by a vacuum pump, and maintaining the negative pressure condition for 15min; sucking the acidic silica sol with the concentration value of 50% into the impregnation tank through a material sucking pipeline preset on the impregnation tank by utilizing the negative pressure environment in the impregnation tank, immersing the acidic silica sol into the first prefabricated braided fabric, and keeping the negative pressure state in the impregnation tank unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining the vacuum pump to pump air to the dipping tank, maintaining the pressure of the dipping tank in a negative pressure state at negative 0.098Mpa for 120min, and closing the vacuum pump to restore the dipping tank to a normal pressure state; opening a cover body of the dipping tank, placing the dipping tank in an oven, setting the temperature in the oven to be 50 ℃ and maintaining until the acidic silica sol is completely changed into a solid state;
step S4: taking out the first prefabricated braided fabric after the dipping treatment from the dipping tank, firstly removing attachments on the surface of the first prefabricated braided fabric, then placing the treated first prefabricated braided fabric in a high-temperature furnace, heating to 450 ℃, and treating for 3 hours under the aerobic condition;
Step S5: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnating tank, pumping air from the impregnating tank through a vacuum pump until the inside of the impregnating tank is pumped, so that the inside of the impregnating tank is in a negative pressure state, the pressure of the negative pressure state is-0.098 Mpa, and maintaining the negative pressure state for 10min; the acidic silica sol with the concentration value of 25% can be sucked into the dipping tank through a preset pumping pipeline on the dipping tank by utilizing the negative pressure state in the dipping tank until the acidic silica sol submerges the first prefabricated braided fabric, and the negative pressure state in the dipping tank is kept unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining a vacuum pump to pump air from the dipping tank, maintaining the negative pressure state of 0.098Mpa of negative pressure in the dipping tank, closing the vacuum pump after 60min, and recovering the inside of the dipping tank to a normal pressure state; opening the cover body of the dipping tank, and taking out the first prefabricated braided fabric;
Step S6: placing the treated first prefabricated braided fabric into an oven, setting the temperature of the oven to 80 ℃, and maintaining the environment at 80 ℃ for 3 hours; transferring the first prefabricated braided fabric into a high-temperature furnace, heating to 450 ℃, and continuously treating for 3 hours under the aerobic condition;
step S7: sequentially repeating the step S5 and the step S6 twice to obtain a prefabricated body;
Step S8: taking out the preform, cleaning attachments on the surface of the preform, controlling a high-temperature furnace to heat to 750 ℃ at a speed of 3 ℃/min, placing the preform in the environment of 750 ℃ for 3 hours, then cooling the high-temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
Example 3
And preparing the revolving body conical quartz composite material according to the target shape and the target size of the quartz composite material.
The preparation method of the quartz composite material comprises the following steps:
Step S1: making a first prefabricated braided fabric: mixing quartz fiber cloth and metal wires in a layering mode, preparing a first prefabricated braided fabric with a flat plate structure by adopting a quartz fiber yarn puncture sewing process, and sequentially processing the first prefabricated braided fabric by adopting the following modes to prepare a prefabricated body; wherein, the technological parameters of the sewing mode are shown in the following table 3;
Step S2: performing a first pre-made braid pretreatment: placing the first prefabricated braided fabric in a high-temperature furnace, and heating the high-temperature furnace to 500 ℃ so that the first prefabricated braided fabric is treated for 3 hours in a high-temperature aerobic environment;
Step S3: dipping treatment: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnation tank, sealing a tank cover of the impregnation tank, pumping air to the inside of the impregnation tank to negative pressure of 0.1Mpa by a vacuum pump, and maintaining the negative pressure condition for 20min; sucking the acidic silica sol with the concentration value of 50% into the impregnation tank through a material sucking pipeline preset on the impregnation tank by utilizing the negative pressure environment in the impregnation tank, immersing the acidic silica sol into the first prefabricated braided fabric, and keeping the negative pressure state in the impregnation tank unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining the vacuum pump to pump air to the dipping tank, maintaining the pressure of the dipping tank in a negative pressure state at negative 0.1Mpa for 120min, closing the vacuum pump, and recovering the dipping tank to a normal pressure state; opening a cover body of the dipping tank, placing the dipping tank in an oven, setting the temperature in the oven to be 50 ℃ and maintaining until the acidic silica sol is completely changed into a solid state;
Step S4: taking out the first prefabricated braided fabric after the dipping treatment from the dipping tank, firstly removing attachments on the surface of the first prefabricated braided fabric, then placing the treated first prefabricated braided fabric in a high-temperature furnace, heating to 500 ℃, and treating for 3 hours under the aerobic condition;
Step S5: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnating tank, pumping air from the impregnating tank through a vacuum pump until the inside of the impregnating tank is pumped, so that the inside of the impregnating tank is in a negative pressure state, the pressure of the negative pressure state is negative 0.1Mpa, and keeping the negative pressure state for 20min; the acidic silica sol with the concentration value of 30% can be sucked into the dipping tank through a preset pumping pipeline on the dipping tank by utilizing the negative pressure state in the dipping tank until the acidic silica sol submerges the first prefabricated braided fabric, and the negative pressure state in the dipping tank is kept unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining a vacuum pump to pump air from the dipping tank, maintaining the negative pressure state of 0.1Mpa of negative pressure in the dipping tank, closing the vacuum pump after 120min, and recovering the inside of the dipping tank to a normal pressure state; opening the cover body of the dipping tank, and taking out the first prefabricated braided fabric;
Step S6: placing the treated first prefabricated braided fabric into an oven, setting the temperature of the oven to be 100 ℃, and maintaining the environment at 100 ℃ for 3 hours; transferring the first prefabricated braided fabric into a high-temperature furnace, heating to 500 ℃, and continuously treating for 3 hours under the aerobic condition;
step S7: sequentially repeating the step S5 and the step S6 twice to obtain a prefabricated body;
Step S8: taking out the preform, cleaning attachments on the surface of the preform, controlling a high-temperature furnace to heat to 800 ℃ at a speed of 3 ℃/min, placing the preform in an environment of 800 ℃ for 3 hours, cooling the high-temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
Comparative example 1
And preparing the tabular quartz composite material according to the target shape and the target size of the quartz composite material.
The preparation method of the quartz composite material comprises the following steps:
Step S1: making a first prefabricated braided fabric: laminating quartz fiber cloth in a layering mode, preparing a first prefabricated braided fabric with a flat plate structure by adopting a quartz fiber yarn puncture sewing process, and sequentially processing the first prefabricated braided fabric in the following mode to prepare a prefabricated body; wherein, the technological parameters of the sewing mode are shown in the following table 4;
Step S2: performing a first pre-made braid pretreatment: placing the first prefabricated braided fabric in a high-temperature furnace, and heating the high-temperature furnace to 500 ℃ so that the first prefabricated braided fabric is treated for 3 hours in a high-temperature aerobic environment;
Step S3: dipping treatment: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnation tank, sealing a tank cover of the impregnation tank, pumping air to the inside of the impregnation tank to negative pressure of 0.1Mpa by a vacuum pump, and maintaining the negative pressure condition for 20min; sucking the acidic silica sol with the concentration value of 50% into the impregnation tank through a material sucking pipeline preset on the impregnation tank by utilizing the negative pressure environment in the impregnation tank, immersing the acidic silica sol into the first prefabricated braided fabric, and keeping the negative pressure state in the impregnation tank unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining the vacuum pump to pump air to the dipping tank, maintaining the pressure of the dipping tank in a negative pressure state at negative 0.1Mpa for 120min, closing the vacuum pump, and recovering the dipping tank to a normal pressure state; opening a cover body of the dipping tank, placing the dipping tank in an oven, setting the temperature in the oven to be 50 ℃ and maintaining until the acidic silica sol is completely changed into a solid state;
Step S4: taking out the first prefabricated braided fabric after the dipping treatment from the dipping tank, firstly removing attachments on the surface of the first prefabricated braided fabric, then placing the treated first prefabricated braided fabric in a high-temperature furnace, heating to 500 ℃, and treating for 3 hours under the aerobic condition;
Step S5: taking out the first prefabricated braided fabric subjected to high-temperature aerobic treatment from the high-temperature furnace, placing the first prefabricated braided fabric in an impregnating tank, pumping air from the impregnating tank through a vacuum pump until the inside of the impregnating tank is pumped, so that the inside of the impregnating tank is in a negative pressure state, the pressure of the negative pressure state is negative 0.1Mpa, and keeping the negative pressure state for 20min; the acidic silica sol with the concentration value of 30% can be sucked into the dipping tank through a preset pumping pipeline on the dipping tank by utilizing the negative pressure state in the dipping tank until the acidic silica sol submerges the first prefabricated braided fabric, and the negative pressure state in the dipping tank is kept unchanged all the time in the process of sucking the acidic silica sol; closing a valve of a pumping pipeline, continuously maintaining a vacuum pump to pump air from the dipping tank, maintaining the negative pressure state of 0.1Mpa of negative pressure in the dipping tank, closing the vacuum pump after 120min, and recovering the inside of the dipping tank to a normal pressure state; opening the cover body of the dipping tank, and taking out the first prefabricated braided fabric;
Step S6: placing the treated first prefabricated braided fabric into an oven, setting the temperature of the oven to be 100 ℃, and maintaining the environment at 100 ℃ for 3 hours; transferring the first prefabricated braided fabric into a high-temperature furnace, heating to 500 ℃, and continuously treating for 3 hours under the aerobic condition;
step S7: sequentially repeating the step S5 and the step S6 twice to obtain a prefabricated body;
Step S8: taking out the preform, cleaning attachments on the surface of the preform, controlling a high-temperature furnace to heat to 800 ℃ at a speed of 3 ℃/min, placing the preform in an environment of 800 ℃ for 3 hours, cooling the high-temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
The three examples and one comparative example obtained above were subjected to performance test in order, and the results are shown in table 5 below.
According to the test methods of flexural strength of fine ceramics (GB/T6569-2006), tensile strength of fine ceramics at room temperature (GB/T23805-2009), compression strength of fiber-reinforced plastics (GB/T1448-2005) and shear strength between fiber-reinforced plastics (GB/T1450.1-2005), the obtained samples were tested for performance, and as can be seen from the above-mentioned Table 5, the quartz composite material prepared by the preparation method of the quartz composite material provided by the application has tensile properties comparable to those of comparative example 1, and in addition, the obtained samples were tested according to the test method of tensile strength of weld joint (GB/T2651-2008), and the tensile strength of weld in comparative example 1 shown in Table 5 was found to be 0MPa or more, while the tensile strength of weld in the quartz composite material prepared in the application was above 18MPa, mainly because the quartz composite material prepared in comparative example 1 could not be well welded with titanium alloy, and the quartz composite material prepared by the application has excellent mechanical properties and the mechanical properties of the application can be well welded with other materials, and the composite materials can be prepared in a special condition and have excellent mechanical properties.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (7)
1. The preparation method of the quartz composite material is characterized by comprising the following steps of:
Step S1: mixing quartz fiber cloth and a wire mesh in a layering manner to obtain a mixed piece, preparing the mixed piece into a first prefabricated braided fabric by utilizing fiber yarns in a sewing manner, sequentially processing the first prefabricated braided fabric in a sewing manner, and preparing a prefabricated body, wherein the wire mesh is paved by wires in a manner that the distance between the wires is 2 mm-4 mm, one layer of the wire mesh is paved between every two layers of quartz fiber cloth to form the mixed piece, the wire is made of any one of TC4 titanium alloy wires and TC6 titanium alloy wires, the diameter of the wire is phi 0.05 mm-0.1 mm, the sewing manner is a lock-type penetration sewing process or a temporary sewing process, and the sewing needle distance of the sewing manner is 4 mm-5 mm;
Step S2: placing the first prefabricated braided fabric in a high-temperature furnace, heating the high-temperature furnace to 450-500 ℃ and maintaining the temperature for 2-4 hours, so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition;
Step S3: taking the first prefabricated braided fabric out of the high-temperature furnace, placing the first prefabricated braided fabric in an impregnation tank, and carrying out impregnation treatment on the first prefabricated braided fabric by using first acidic silica sol, wherein the concentration of the first acidic silica sol is 45% -50%;
Step S4: placing the dipping tank in an oven, setting the temperature of the oven at 40-60 ℃ and maintaining until the first acidic silica sol is completely changed into a solid state;
step S5: taking the first prefabricated braided fabric out of the dipping tank and placing the first prefabricated braided fabric in the high-temperature furnace, and heating the high-temperature furnace to 400-500 ℃ so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high-temperature condition;
step S6: taking the first prefabricated braided fabric out of the high-temperature furnace, placing the first prefabricated braided fabric in an impregnation tank, and carrying out impregnation treatment on the first prefabricated braided fabric by using second acidic silica sol, wherein the concentration of the second acidic silica sol is 25% -40%;
step S7: placing the first prefabricated braided fabric in an oven, setting the temperature of the oven to be 70-100 ℃, and keeping the first prefabricated braided fabric at 70-100 ℃ for 2-4 hours; transferring the first prefabricated braided fabric into the high temperature furnace, heating the high temperature furnace to 400-500 ℃ and maintaining the temperature for 2-4 hours, so that the first prefabricated braided fabric is treated for 2-4 hours under the aerobic high temperature condition;
step S8: repeating the step S6 and the step S7 at least twice to obtain the prefabricated body;
Step S9: taking out the preform and placing the preform in the high-temperature furnace, controlling the high-temperature furnace to heat to 700-800 ℃ at 2-4 ℃/min, placing the preform in the environment of 700-800 ℃ for 3-4 h, then cooling the high-temperature furnace to room temperature, and taking out the preform to obtain the quartz composite material.
2. The method for producing a quartz composite material according to claim 1,
The dipping tank is provided with a pumping pipeline for sucking the first acidic silica sol or the second acidic silica sol into the dipping tank;
in addition, the step S3 further includes the following steps:
step S31: pumping air from the interior of the dipping tank through a vacuum pump so as to enable the interior of the dipping tank to be in a negative pressure state, and keeping the negative pressure state for 10-20 min;
Step S32: sucking the first acidic silica sol into the impregnation tank through the material sucking pipeline, immersing the first prefabricated braided fabric in the first acidic silica sol, and keeping the negative pressure state in the impregnation tank unchanged all the time in the process of sucking the first acidic silica sol;
step S33: closing the pumping pipeline, and continuously maintaining the vacuum pump to continuously pump the impregnating tank so as to maintain the impregnating tank in a negative pressure state for 60-120 min;
step S34: and closing the vacuum pump to restore the inside of the dipping tank to a normal pressure state.
3. A method for producing a quartz composite material according to claim 1 or 2, characterized in that,
The fiber yarn has a tex value of any one of 570, 190 and 195.
4. A method of preparing a quartz composite material as defined in claim 3,
The quartz fiber cloth is a quartz glass fiber satin cloth with the thickness of 0.1 mm-0.3 mm.
5. The method for producing a quartz composite material according to claim 2, wherein,
The pressure of the negative pressure state is negative 0.095 MPa-0.1 MPa.
6. The method for preparing a quartz composite material according to claim 5,
The first prefabricated braided fabric is in a flat plate shape, a rotary body cone shape or a special-shaped structure shape.
7. A quartz composite material prepared by the method of preparing a quartz composite material according to any of claims 1-6, for use in welding metal parts secured to the exterior.
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