CN113185327B - Silicon carbide whisker obtained on surface of carbon fiber reinforced composite material rapidly and efficiently and preparation method thereof - Google Patents
Silicon carbide whisker obtained on surface of carbon fiber reinforced composite material rapidly and efficiently and preparation method thereof Download PDFInfo
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- CN113185327B CN113185327B CN202110470308.2A CN202110470308A CN113185327B CN 113185327 B CN113185327 B CN 113185327B CN 202110470308 A CN202110470308 A CN 202110470308A CN 113185327 B CN113185327 B CN 113185327B
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- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The invention provides a silicon carbide whisker obtained on the surface of a carbon fiber reinforced composite material quickly and efficiently and a preparation method thereof, wherein the silicon carbide whisker is obtained by pretreating a low-density carbon felt in a mixture consisting of silicon powder, graphite powder and a resin alcohol solution, putting a carbon fiber reinforced composite material block into an interlayer of the pretreated carbon felt at a lower temperature, and growing an obtained product on each surface of the carbon fiber reinforced composite material after temperature treatment. The method has the advantages of low cost, low requirement on equipment, simple and convenient process flow and the like, can quickly and efficiently prepare a large amount of SiC whiskers on the surface of the carbon fiber reinforced composite material, and has high whisker growth efficiency and uniform distribution of the generated whiskers.
Description
Technical Field
The invention relates to a method for quickly and efficiently obtaining silicon carbide whiskers on the surface of a carbon fiber reinforced composite material and a preparation method thereof.
Background
At present, carbon fiber reinforced carbon-based (C/C) and silicon carbide-based (C/SiC) composite materials have the advantages of low density, high specific strength-specific modulus, high temperature resistance and the like, are widely applied to the field of aerospace, and become main materials of light structures and heat release structures. However, the carbon-based material is easily oxidized in an oxygen environment at a temperature of more than 400 ℃, so that the carbon fiber or the carbon matrix is oxidized and lost, the mechanical property of the composite material is greatly damaged, and the safety of the component is influenced. Therefore, there is a need for an oxidation resistant protection for carbon fiber reinforced composites. The protection of the composite material by preparing the ceramic coating on the surface of the carbon fiber reinforced composite material is the most common mode at present, but the ceramic coating has low toughness, and the prepared ceramic coating is easy to generate defects of holes, cracks and the like due to the limitation of the preparation process, so that the protection effect of the ceramic coating is reduced. The SiC whisker toughened ceramic coating can improve the quality of the coating and improve the toughness of the coating, and is widely researched at present.
At present, there are two main aspects for preparing SiC whiskers, one is a normal pressure Chemical Vapor Deposition (CVD) method, and the other is a carbothermic method. The normal pressure CVD method is that the sample soaked with the catalyst is put into a tube furnace, the furnace body is vacuumized and protective gas is introduced to the normal pressure state, and then SiC precursor and carrier gas are introduced into the furnace body to react to generate SiC whisker after the temperature is reached. The method has high requirements on equipment, needs several paths of gas to be introduced into the equipment, and the precursor is generally corrosive, so that the equipment is corroded, and the maintenance cost of the equipment is high. On the other hand, the generated SiC whiskers are not very uniform, enrichment regions are easy to generate on a matrix, and the uniformity of all surfaces cannot be achieved. The other method is a carbothermic method, which makes the raw material generate Si steam or SiO gas at high temperature, and directly reacts with carbon on the surface of the composite material to generate SiC whiskers. The temperature of the method needs to be higher than the melting point of silicon, the requirement on equipment is high, and the method can only generate SiC whiskers on one surface basically, so that the problem that the SiC whiskers are generated on the whole surface of the composite material is difficult.
Disclosure of Invention
According to the normal pressure CVD method, the requirement on equipment is high, a plurality of paths of gases are needed to be introduced into the equipment, a precursor is generally corrosive, the equipment is corroded, the equipment maintenance cost is high, on the other hand, the generated SiC crystal whiskers are not uniform, enrichment areas are easy to generate on a substrate, and all surfaces cannot be uniform; the temperature of the carbothermic method needs to be higher than the melting point of silicon, the requirement on equipment is high, and the method can only generate SiC whiskers on one surface basically, so that the problem that the generation of SiC whiskers on the whole surface of the composite material is difficult is solved. The method mainly comprises the steps of treating the carbon felt with low density, silicon powder and graphite powder, and then putting the carbon fiber reinforced composite material block into the interlayer of the carbon felt at a lower temperature, so as to grow SiC whiskers on each surface of the carbon fiber reinforced composite material, and has the advantages of low cost, low requirement on equipment, simple and rapid process and the like.
The technical means adopted by the invention are as follows:
the silicon carbide whisker is obtained on the surface of a carbon fiber reinforced composite material quickly and efficiently, and is an obtained product which is obtained by pretreating a low-density carbon felt in a mixture consisting of silicon powder, graphite powder and a resin alcohol solution, putting a carbon fiber reinforced composite material block into an interlayer of the pretreated carbon felt at a lower temperature, and growing on each surface of the carbon fiber reinforced composite material after temperature treatment.
The invention also provides a preparation method for quickly and efficiently obtaining the silicon carbide whiskers on the surface of the carbon fiber reinforced composite material, which comprises the following steps:
s1, pretreatment of raw materials:
s11, selecting a carbon fiber reinforced composite material as a substrate, and polishing the surface of the substrate by using sand paper for later use;
s12, mixing silicon powder and graphite powder in a resin alcohol solution with the mass content of 25% -50% according to the mass ratio of 1:4-4:1 to form a mixture;
s13, cutting the low-density carbon felt into a certain size, and immersing the carbon felt into the mixture for 5-20 minutes;
s14, taking out the carbon felt processed in the step S13, and drying the carbon felt in a drying oven for 2 hours at 100 ℃ after the alcohol is completely volatilized; then the resin is decomposed by heat preservation for 1 hour at 600 ℃ in a tube furnace;
s15, soaking the carbon felt processed in the step S14 in a salt solution of catalyst metal with the content of 0.05-0.20mol/L for 2 hours, and then taking out and drying for later use;
s2, preparation of SiC whiskers:
s21, preparing a sample: taking two carbon felts pretreated in the step S1 and a substrate pretreated in the step S1, placing the first carbon felt at the bottom, placing the substrate on the first carbon felt, and covering the second carbon felt above the substrate;
s22, placing the sample prepared in the step S21 in a graphite crucible, and placing the graphite crucible in a heat treatment furnace;
s23, primarily vacuumizing the furnace body of the treatment furnace, filling argon to normal pressure for protection after vacuumizing is completed, and then carrying out stepwise heating to 1100-1300 ℃ and then carrying out heat preservation for 2 hours; then cooling;
and S24, when the temperature is reduced to the room temperature, taking out the sample from the furnace body, and carefully taking out the prepared sample to obtain the SiC whiskers uniformly covered on the surface of the composite material.
Further, in the step S11, the size of the substrate is 10mm × 10mm × 10 mm.
Further, in the step S12, the mass ratio of the powder to the resin alcohol solution in the mixture is 1:4 to 4: 1.
Further, in the step S13, the density of the carbon felt is 0.4-1.0g/cm3。
Further, in the step S13, the cut carbon felt has a size of 50mm × 50mm × 10 mm.
Further, in step S15, the salt solution of the catalyst metal is a nickel sulfate solution, a ferric sulfate solution, or a nickel nitrate solution.
Further, in step S23, the temperature is raised in a stepwise manner at a temperature of 10 ℃/min.
Compared with the prior art, the invention has the following advantages:
1. compared with the existing preparation process, the method for quickly and efficiently obtaining the silicon carbide whiskers on the surface of the carbon fiber reinforced composite material and the preparation method thereof have the characteristics of simple and convenient process flow, high whisker growth efficiency and uniform distribution of the generated whiskers. Can prepare a large amount of SiC whiskers rapidly and reduce the cost at the same time.
2. According to the method for quickly and efficiently obtaining the silicon carbide whiskers on the surface of the carbon fiber reinforced composite material and the preparation method thereof, the carbon felt with low density, the silicon powder and the graphite powder are treated, and the carbon fiber reinforced composite material block is placed in the interlayer of the carbon felt at a low temperature, so that the SiC whiskers grow on each surface of the carbon fiber reinforced composite material. Has the advantages of low cost, low requirement on equipment, simple and quick process and the like.
3. According to the silicon carbide whisker obtained on the surface of the carbon fiber reinforced composite material rapidly and efficiently and the preparation method thereof provided by the invention, the SiC whisker can be prepared on the surface of the carbon fiber reinforced composite material rapidly and efficiently, the dependence of the preparation of the SiC whisker on equipment is reduced, the cost for preparing the SiC whisker is reduced, the prepared SiC whisker can be better covered on the surface of the composite material, and the whisker is more uniform.
In conclusion, the technical scheme of the invention can solve the problems that the normal pressure CVD method in the prior art has higher requirements on equipment, needs a plurality of paths of gas to be introduced into the equipment, and the precursor is generally corrosive, so that the equipment is corroded, the equipment maintenance cost is higher, on the other hand, the generated SiC whiskers are not uniform, enrichment regions are easy to generate on a substrate, and all surfaces cannot be uniform; the temperature of the carbothermic method needs to be higher than the melting point of silicon, the requirement on equipment is high, and the method can only generate SiC whiskers on one surface basically, so that the problem that the SiC whiskers are difficult to generate on the whole surface of the composite material is solved.
Based on the reasons, the invention can be widely popularized in the fields of ceramics, ceramic coating preparation and the like.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic diagram of a sample of SiC whiskers prepared according to the present invention.
FIG. 2 is a schematic view of the microstructure of the SiC whisker of the invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. 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.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
The SiC whiskers have very outstanding advantages in the aspects of reducing the defects of the ceramic coating and improving the quality and the toughness of the ceramic coating. As shown in fig. 1-2, the silicon carbide whisker obtained on the surface of the carbon fiber reinforced composite material in the invention is obtained quickly and efficiently, and is obtained by pretreating a low-density carbon felt in a mixture of silicon powder, graphite powder and a resin alcohol solution, placing a carbon fiber reinforced composite material block into an interlayer of the pretreated carbon felt at a lower temperature, and growing on each surface of the carbon fiber reinforced composite material after temperature treatment.
The invention provides a preparation method for quickly and efficiently obtaining silicon carbide whiskers on the surface of a carbon fiber reinforced composite material, which comprises the following steps:
firstly, pretreatment of raw materials
1. The carbon fiber reinforced composite material is selected as a matrix, and the size is 10mm multiplied by 10 mm. And (3) polishing the surface of the substrate by using sand paper for later use.
2. Silicon powder and graphite powder are mixed in a resin alcohol solution with the mass content of 25% according to the mass ratio of 1: 4. The mass ratio of the powder to the resin alcohol solution was 1:4 (powder means silicon powder and graphite powder).
3. The density is 0.7g/cm3The carbon felt was cut into a size of 50mm × 50mm × 10mm, and the carbon felt was immersed in a resin alcohol solution of silica powder and graphite powder for 5 minutes.
4. Taking out the carbon felt, and drying in a drying oven at 100 ℃ for 2 hours after the alcohol is completely volatilized. The resin was then decomposed in a tube oven at 600 ℃ for 1 hour.
5. Soaking the carbon felt in a nickel sulfate solution or a nickel nitrate solution with the content of 0.05mol/L for 2 hours, and then taking out and drying for later use.
Preparation of SiC crystal whisker
1. Preparing a sample: placing a prepared carbon felt at the bottom, placing the prepared carbon fiber reinforced composite material on the carbon felt, and covering another carbon felt on the carbon fiber reinforced composite material.
2. The prepared sample was placed in a graphite crucible, and the graphite crucible was placed in a heat treatment furnace.
3. Primarily vacuumizing a furnace body of the heat treatment furnace, then filling argon to normal pressure for protection, carrying out step-type temperature rise according to the temperature of 10 ℃/min, and carrying out heat preservation when the temperature rises to a certain temperature of 1100-1300 ℃, wherein the heat preservation time is 2 hours. Then the temperature is reduced (to room temperature).
4. When the temperature is reduced to the room temperature, the sample is taken out from the furnace body, the prepared sample is carefully taken out, and the SiC whiskers are uniformly covered on the surface of the composite material, so that the SiC whiskers growing on each surface of the carbon fiber reinforced composite material are obtained.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A preparation method for quickly and efficiently obtaining silicon carbide whiskers on the surface of a carbon fiber reinforced composite material is characterized in that a low-density carbon felt is pretreated in a mixture consisting of silicon powder, graphite powder and a resin alcohol solution, a carbon fiber reinforced composite material block is placed in an interlayer of the pretreated carbon felt at a lower temperature, and products are grown on the surfaces of the carbon fiber reinforced composite material after temperature treatment;
the preparation method is characterized by comprising the following steps:
s1, pretreatment of raw materials:
s11, selecting a carbon fiber reinforced composite material as a substrate, and polishing the surface of the substrate by using sand paper for later use;
s12, mixing silicon powder and graphite powder in a resin alcohol solution with the mass content of 25% -50% according to the mass ratio of 1:4-4:1 to form a mixture;
s13, cutting the low-density carbon felt into a certain size, and immersing the carbon felt into the mixture for 5-20 minutes;
s14, taking out the carbon felt processed in the step S13, and drying the carbon felt in a drying oven for 2 hours at 100 ℃ after the alcohol is completely volatilized; then the resin is decomposed by heat preservation for 1 hour at 600 ℃ in a tube furnace;
s15, soaking the carbon felt processed in the step S14 in a salt solution of catalyst metal with the content of 0.05-0.20mol/L for 2 hours, and then taking out and drying for later use;
s2, preparation of SiC whiskers:
s21, preparing a sample: taking two carbon felts pretreated in the step S1 and a substrate pretreated in the step S1, placing the first carbon felt at the bottom, placing the substrate on the first carbon felt, and covering the second carbon felt above the substrate;
s22, placing the sample prepared in the step S21 in a graphite crucible, and placing the graphite crucible in a heat treatment furnace;
s23, primarily vacuumizing the furnace body of the treatment furnace, filling argon to normal pressure for protection after vacuumizing is completed, and then carrying out stepwise heating to 1100-1300 ℃ and then carrying out heat preservation for 2 hours; then cooling;
and S24, when the temperature is reduced to the room temperature, taking out the sample from the furnace body, and carefully taking out the prepared sample to obtain the SiC whiskers uniformly covered on the surface of the composite material.
2. The method for preparing silicon carbide whiskers on the surface of a carbon fiber reinforced composite material in a rapid and efficient manner according to claim 1, wherein in the step S11, the size of the matrix is 10mm by 10 mm.
3. The method for preparing silicon carbide whiskers on the surface of a carbon fiber reinforced composite material in a rapid and efficient manner according to claim 1, wherein in the step S12, the mass ratio of the powder to the resin alcohol solution in the mixture is 1:4-4: 1.
4. The method for preparing silicon carbide whiskers on the surface of a carbon fiber reinforced composite material in a rapid and efficient manner according to claim 1, wherein in the step S13, the density of the carbon felt is 0.4-1.0g/cm3。
5. The method for preparing silicon carbide whiskers on the surface of a carbon fiber reinforced composite material in a rapid and efficient manner according to claim 1 or 4, wherein in the step S13, the cut carbon felt has a size of 50mm x 10 mm.
6. The method for preparing silicon carbide whiskers on the surface of a carbon fiber reinforced composite material in a rapid and efficient manner according to claim 1, wherein in step S15, the salt solution of the catalyst metal is a nickel sulfate solution, a ferric sulfate solution or a nickel nitrate solution.
7. The method for rapidly and efficiently preparing silicon carbide whiskers on the surface of a carbon fiber reinforced composite material according to claim 1, wherein in the step S23, the temperature is increased in a stepwise manner at a temperature of 10 ℃/min.
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