CN113912416A - Method for recycling silicon carbide fibers and application - Google Patents
Method for recycling silicon carbide fibers and application Download PDFInfo
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- CN113912416A CN113912416A CN202111330001.9A CN202111330001A CN113912416A CN 113912416 A CN113912416 A CN 113912416A CN 202111330001 A CN202111330001 A CN 202111330001A CN 113912416 A CN113912416 A CN 113912416A
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract
The invention relates to a method for recycling silicon carbide fiber and application thereof, which mainly aims at the prepreg-infiltration process for preparing a silicon carbide fiber reinforced silicon carbide composite material.
Description
Technical Field
The invention relates to a method for recycling silicon carbide fibers and application thereof, mainly aiming at recycling waste fibers, prepreg, cured preform and fibers in a carbonized porous body generated in the process of preparing a silicon carbide fiber reinforced silicon carbide composite material by a prepreg-infiltration process, and belongs to the field of composite materials.
Background
The preparation method of the silicon carbide fiber reinforced silicon carbide composite material by the prepreg-infiltration process mainly comprises the steps of fiber interface layer deposition, prepreg preparation, hot press molding, carbonization and infiltration. In each of the above steps, there is a waste problem. In the interface layer deposition step, waste silk such as uneven interface layer deposition or broken silk and broken silk exists. The prepreg mainly comprises silicon carbide fiber and resin, is an intermediate material for preparing the silicon carbide fiber reinforced silicon carbide composite material by a prepreg-infiltration process, can generate more leftover materials in the preparation process of parts, and also has overdue or deteriorated prepreg in the storage process. Thirdly, hot-press forming is a process of curing resin by the laid prepreg according to a certain temperature and pressure, and waste products generated in the process mainly comprise silicon carbide fibers and the cured resin. And fourthly, the carbonization step is to crack the prefabricated body after hot press forming at high temperature to obtain the fiber reinforced porous body, and waste products caused by bulging, layering and the like exist in the process. The waste products produced in the preparation processes are usually treated in the form of industrial wastes, and the silicon carbide fibers and the resin cannot be completely degraded, so that certain pollution is caused to the environment. In addition, because the silicon carbide fiber has low density and thin diameter, the silicon carbide fiber can easily fly with wind, and the modulus of the silicon carbide fiber is high, so that garbage disposal personnel can be easily injured. Meanwhile, the price of the silicon carbide fiber raw material is usually 5-8 ten thousand yuan/kg, the price of the fiber containing the interface layer is higher, the fiber has excellent oxidation resistance, and the fiber is also a great waste when being directly used as industrial garbage treatment.
Disclosure of Invention
The invention provides a method for recycling silicon carbide fibers and application thereof aiming at solving the problems, and aims to recycle fibers with interface layers, prepregs, cured preforms and carbonized porous bodies generated in the process of preparing silicon carbide fiber reinforced silicon carbide composite materials by a prepreg-infiltration process.
The purpose of the invention is realized by the following technical scheme:
the method for recycling the silicon carbide fiber provided by the invention comprises the following steps:
step one, high-temperature oxidation
Placing silicon carbide waste wires, prepreg, preform and fiber reinforced porous body generated in the process of depositing the interface layer as raw materials in an oxidation furnace, heating to 900-1000 ℃ and keeping for 1 hour to remove resin or carbon to obtain silicon carbide fiber;
step two, fiber shearing
Shearing the silicon carbide fiber obtained in the step one to obtain a short-cut silicon carbide fiber, wherein the length of the sheared fiber is less than 10 mm;
step three, mixing the materials
Mixing the chopped silicon carbide fibers obtained in the step two with infiltration powder, an adhesive and a solvent, and carrying out ball milling for 2-5 hours, wherein the mass parts of the chopped silicon carbide fibers are as follows:
the infiltration powder is one or a mixture of silicon powder and metal powder;
the selection mode of the adhesive and the corresponding solvent is one of the following modes:
the first method comprises the following steps: the adhesive is an aqueous adhesive, and the solvent is water;
and the second method comprises the following steps: the solvent is an organic solvent, and the selected adhesive can be dissolved in the organic solvent;
step four, suction filtration shaping
Pouring the mixture obtained in the third step into a suction filter with the surface covered with filter paper, carrying out suction filtration for 5-10 hours to remove water, and carrying out shaping to obtain a pre-shaped body;
step five, drying treatment
Placing the pre-shaped body in a drying oven for drying, wherein the drying temperature is 60-120 ℃, and the drying time is 3-5 hours, so as to obtain a dried pre-shaped body;
step six, sintering and shaping
And (3) placing the dried pre-shaped body in a high-temperature furnace for sintering, wherein the sintering atmosphere is argon, the sintering temperature is 1350-1500 ℃, and the duration is 30-60 min, so as to obtain the chopped silicon carbide fiber felt body with the porous structure.
In one implementation, the raw material in the first step is waste fiber filaments generated in the production, weaving or other process of preparing the composite material by using the silicon carbide fibers.
In one implementation, the aqueous adhesive in step three is polyvinyl alcohol adhesive resin, ethylene acetate aqueous adhesive, or epoxy aqueous adhesive.
In one embodiment, the aqueous adhesive in step three is a rubber-based aqueous adhesive.
In one embodiment, the organic solvent in step three is ethanol, toluene or xylene.
In one implementation, the particle size of the silicon powder in the third step is 0.5-50 μm, and the selection of the particle size can be better and uniformly mixed with the chopped silicon carbide fiber;
in one embodiment, the metal powder in step three is titanium, zirconium, hafnium.
The technical scheme of the invention also provides an application of the chopped silicon carbide fiber felt body with the porous structure prepared from the recycled silicon carbide fiber, and the chopped silicon carbide fiber felt body with the porous structure is used for high-temperature filtration or is made into a crucible cover of a graphite crucible for fused siliconizing. The crucible cover prepared by the material has the following advantages: because the fibers are recycled fibers and the interface layer for protecting the fibers is arranged on the surfaces of the fibers, the fiber can resist the corrosion of the gaseous silicon and has long service life; due to the porous structure, the graphite crucible has good air permeability, and meets the air permeability requirement during vacuum infiltration of the graphite crucible.
According to the technical scheme, waste products generated in the process of preparing the silicon carbide fiber reinforced silicon carbide composite material by the prepreg-infiltration process are subjected to high-temperature oxidation to remove resin or carbon to obtain silicon carbide fibers containing an interface layer, the fibers are further sheared, mixed with infiltration powder and an adhesive, subjected to suction filtration and preliminary shaping, and then dried and sintered to obtain the silicon carbide fiber shaped body with the porous structure. The shaped body can be used as a crucible cover in a vacuum infiltration step to replace a graphite crucible cover with holes.
The advantages and features of the technical scheme of the invention are summarized as follows:
1. the waste materials generated in each step of preparing the composite material by the prepreg-infiltration process cause great pollution to the environment, and are easy to cause damage to garbage disposal personnel due to small diameter and high hardness, and the disposal difficulty is great. The invention can realize the recycling of the silicon carbide fiber, thereby reducing the pressure of environmental pollution;
2. the price of the silicon carbide fiber raw material is usually 5-8 ten thousand yuan/kg, the price of the fiber containing the interface layer is higher, the fiber has excellent oxidation resistance, and the fiber is also extremely wasted when being directly used as industrial garbage treatment. The recovery of the invention enables the excellent performance of the silicon carbide to be reused, thereby effectively reducing the resource waste.
3. Adopt graphite crucible usually during melting siliconizing, the siliconizing process is vacuum process usually, consequently for guaranteeing the inside higher vacuum degree that reaches of crucible, need cover the processing of punching on the crucible, and during high temperature melting siliconizing, because volatilizing of silicon vapour, cause the graphite lid to receive the erosion easily, consequently change the frequency higher. The crucible cover prepared by the recycled silicon carbide fiber can bear the erosion of the gas silicon due to the interface layer protection on the surface of the fiber, so that the service life is prolonged, and the high vacuum degree in the crucible can be ensured due to the porous structure.
4. According to the invention, silicon is used as a high-temperature binder to bond fibers together, so that a pollution source can be prevented from being introduced in the siliconizing process; because the silicon alloy with the melting point lower than that of pure silicon is usually adopted in the melting siliconizing process, the silicon in the crucible cover can be ensured not to melt in the siliconizing process, and certain strength is kept. The content of silicon powder needs to be strictly controlled in the preparation process, the gas permeability of the prepared crucible cover is easy to be insufficient due to excessively high addition amount, and the strength of the crucible cover is insufficient due to excessively low addition amount.
5. The invention adopts the suction filtration method for shaping, has lower requirement on equipment and has convenient and practical effects on the crucible cover with simpler shape.
6. The equipment is simple, and for a unit adopting the prepreg-infiltration process to prepare the composite material, the silicon carbide fiber can be recycled only by adding the oxidation furnace and the corresponding suction filtration device, so that the investment scale is small, and the income is high.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific examples:
example 1
The method for recycling the silicon carbide fiber comprises the following steps:
(1) treating the silicon carbide fiber prepreg in an oxidation furnace at 1000 ℃ for 1 hour, and removing resin or carbon to obtain silicon carbide fiber;
(2) shearing the obtained silicon carbide fiber, wherein the length after shearing is less than 10mm, and obtaining the chopped silicon carbide fiber;
(3) and mixing the chopped silicon carbide fibers obtained in the step with silicon powder, polyvinyl alcohol adhesive resin and water, and carrying out ball milling for 5 hours. Wherein: the weight of the chopped silicon carbide fiber is 1000g, the weight of silicon powder with the particle size of 10 mu m is 300g, the weight of the polyvinyl alcohol adhesive resin is 100g, and the weight of water is 3000 g;
(4) pouring the slurry obtained in the above step into a suction filter with the diameter of 200mm and the surface covered with filter paper, and carrying out suction filtration for 5 hours to remove water, thereby obtaining a preset body.
(5) And (3) drying the pre-shaped body in an oven at the drying temperature of 100 ℃ for 3 hours to obtain the dried pre-shaped body.
(6) And (3) sintering the dried pre-shaped body prepared in the step in a high-temperature furnace, wherein the sintering atmosphere is argon, the sintering temperature is 1450 ℃, and the duration is 30min, so that the silicon carbide fiber shaped body with the porous structure and the diameter of 200mm and the thickness of 22mm is obtained.
Example 2
The method for recycling the silicon carbide fiber comprises the following steps:
(1) treating the silicon carbide fiber prepreg in an oxidation furnace at 1000 ℃ for 1 hour, and removing resin or carbon to obtain silicon carbide fiber;
(2) shearing the obtained silicon carbide fiber, wherein the length after shearing is less than 10mm, and obtaining the chopped silicon carbide fiber;
(3) and mixing the chopped silicon carbide fibers obtained in the step with silicon powder, polyvinyl alcohol adhesive resin and water, and carrying out ball milling for 5 hours. Wherein: the weight of the chopped silicon carbide fiber is 1000g, the weight of silicon powder with the particle size of 10 mu m is 300g, the weight of the polyvinyl alcohol adhesive resin is 100g, and the weight of water is 3000 g;
(4) pouring the slurry obtained in the step into a suction filter with the size of 200 multiplied by 200mm and the surface covered with filter paper, and carrying out suction filtration for 5 hours to remove water to obtain a pre-formed body;
(5) placing the pre-shaped body in an oven for drying, wherein the drying temperature is 100 ℃, and the drying time is 3 hours, so as to obtain a dried pre-shaped body;
(6) and (3) sintering the dried pre-shaped body prepared in the step in a high-temperature furnace, wherein the sintering atmosphere is argon, the sintering temperature is 1450 ℃, and the duration is 30min, so that the silicon carbide fiber shaped body with the porous structure and the diameter of 200 x 10mm is obtained.
Example 3
The method for recycling the silicon carbide fiber comprises the following steps:
(1) treating the silicon carbide fiber prepreg in an oxidation furnace at 1000 ℃ for 1 hour, and removing resin or carbon to obtain silicon carbide fiber;
(2) shearing the obtained silicon carbide fiber, wherein the length after shearing is less than 10mm, and obtaining the chopped silicon carbide fiber;
(3) and mixing the chopped silicon carbide fibers obtained in the step with silicon powder, water-based epoxy resin and water, and performing ball milling for 3 hours. Wherein: the weight of the chopped silicon carbide fiber is 1000g, the weight of silicon powder with the particle size of 10 mu m is 300g, the weight of the water-based epoxy resin is 150g, and the weight of water is 3500 g;
(4) pouring the slurry obtained in the step into a suction filter with the diameter of 200mm and the surface covered with filter paper, and carrying out suction filtration for 3 hours to remove water to obtain a preset body;
(5) placing the pre-shaped body in an oven for drying, wherein the drying temperature is 80 ℃, and the drying time is 3 hours, so as to obtain a dried pre-shaped body;
(6) and (3) sintering the dried pre-shaped body prepared in the step in a high-temperature furnace, wherein the sintering atmosphere is argon, the sintering temperature is 1450 ℃, and the duration is 30min, so that the silicon carbide fiber shaped body with the porous structure and the diameter of 200mm and the thickness of 22mm is obtained.
Claims (8)
1. A method for recycling silicon carbide fibers is characterized by comprising the following steps: the method comprises the following steps:
step one, high-temperature oxidation
Placing silicon carbide waste filaments, prepreg, preform and fiber reinforced porous body which are generated in the process of depositing the interface layer as raw materials in an oxidation furnace, heating to 900-1000 ℃ and keeping for 1 hour to obtain silicon carbide fiber;
step two, fiber shearing
Shearing the silicon carbide fiber obtained in the step one to obtain a short-cut silicon carbide fiber, wherein the length of the sheared fiber is less than 10 mm;
step three, mixing the materials
Mixing the chopped silicon carbide fibers obtained in the step two with infiltration powder, an adhesive and a solvent, and carrying out ball milling for 2-5 hours, wherein the mass parts of the chopped silicon carbide fibers are as follows:
the infiltration powder is one or a mixture of silicon powder and metal powder;
the selection mode of the adhesive and the corresponding solvent is one of the following modes:
the first method comprises the following steps: the adhesive is an aqueous adhesive, and the solvent is water;
and the second method comprises the following steps: the solvent is an organic solvent, and the selected adhesive can be dissolved in the organic solvent;
step four, suction filtration shaping
Pouring the mixture obtained in the third step into a suction filter with the surface covered with filter paper, carrying out suction filtration for 5-10 hours to remove water, and carrying out shaping to obtain a pre-shaped body;
step five, drying treatment
Placing the pre-shaped body in a drying oven for drying, wherein the drying temperature is 60-120 ℃, and the drying time is 3-5 hours, so as to obtain a dried pre-shaped body;
step six, sintering and shaping
And (3) placing the dried pre-shaped body in a high-temperature furnace for sintering, wherein the sintering atmosphere is argon, the sintering temperature is 1350-1500 ℃, and the duration is 30-60 min, so as to obtain the chopped silicon carbide fiber felt body with the porous structure.
2. The method of claim 1, wherein the silicon carbide fiber is recycled by: in the first step, the raw material is waste fiber filament generated in the production, weaving or other process methods of the silicon carbide fiber for preparing the composite material.
3. The method of claim 1, wherein the silicon carbide fiber is recycled by: the aqueous adhesive in the third step is polyvinyl alcohol adhesive resin, ethylene acetate aqueous adhesive and epoxy aqueous adhesive.
4. The method of claim 1, wherein the silicon carbide fiber is recycled by: the water-based adhesive in the third step is rubber water-based adhesive.
5. The method of claim 1, wherein the silicon carbide fiber is recycled by: the organic solvent in the third step is ethanol, toluene or xylene.
6. The method of claim 1, wherein the silicon carbide fiber is recycled by: the particle size of the silicon powder in the third step is 0.5-50 μm.
7. The method of claim 1, wherein the silicon carbide fiber is recycled by: the metal powder in the third step is titanium, zirconium and hafnium.
8. The use of the chopped silicon carbide fiber mat body of claim 1, which is prepared from recycled silicon carbide fibers and has a porous structure, wherein the chopped silicon carbide fiber mat body comprises: the chopped silicon carbide fiber felt with the porous structure is used for high-temperature filtration or is made into a crucible cover of a graphite crucible for melt siliconizing.
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