CN115745642B - Chopped fiber reinforced boron carbide ceramic sheet and preparation method and application thereof - Google Patents
Chopped fiber reinforced boron carbide ceramic sheet and preparation method and application thereof Download PDFInfo
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- CN115745642B CN115745642B CN202211459048.XA CN202211459048A CN115745642B CN 115745642 B CN115745642 B CN 115745642B CN 202211459048 A CN202211459048 A CN 202211459048A CN 115745642 B CN115745642 B CN 115745642B
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Abstract
The invention discloses a chopped fiber reinforced boron carbide ceramic sheet, a preparation method and application thereof. The preparation method can maintain the integrity of the length of the chopped fiber in the final material so as to ensure the reinforcing and toughening effects.
Description
Technical Field
The invention relates to the technical field of ceramic sheets, in particular to a chopped fiber reinforced boron carbide ceramic sheet and a preparation method and application thereof.
Background
Boron carbide has low density, high modulus and high hardness, so that the boron carbide becomes a main material for military armor and space application. The single-phase boron carbide ceramic has low fracture toughness and poor external impact load resistance, and limits the exertion of anti-elastic performance. The carbon fiber has the comprehensive properties of high temperature resistance, low density, high strength and the like, and the boron carbide composite material prepared by the reinforced fiber has the advantages of high strength, high toughness, high hardness, good shock resistance and the like compared with the unidirectional boron carbide ceramic, and can improve the multiple striking resistance of the bulletproof material and the bulletproof performance of the bulletproof plate.
The existing short fiber reinforced boron carbide ceramic material is prepared by mixing and ball milling short carbon fibers, boron carbide powder and corresponding dispersing agents and adopting a hot pressing or reaction sintering process, wherein the short carbon fibers in the prepared composite material are greatly damaged due to the ball milling, hot pressing and other processes, and the retention length of the fibers in the composite material is only 50-250 micrometers, so that the reinforcing and toughening effects of the composite material are obviously reduced.
Disclosure of Invention
The invention provides a chopped fiber reinforced boron carbide ceramic sheet and a preparation method and application thereof, which are used for overcoming the defects of poor reinforcing and toughening effects and the like caused by the damage of fiber length in the prior art.
In order to achieve the above object, the present invention provides a method for preparing a chopped fiber reinforced boron carbide ceramic sheet, which is characterized by comprising the following steps:
s1: weighing chopped fibers and a mixed solution I according to a mass ratio of 1:50-1:100, and uniformly mixing to obtain slurry A; the mixed solution I is 0.5-2% of polyacrylamide aqueous solution or hydroxymethyl cellulose sodium aqueous solution; the two dispersants are soluble in water, so that the method is economical and environment-friendly; in addition, the aqueous solution with low concentration of the two dispersing agents has higher viscosity, can well disperse fibers, and is not easy to settle for a long time. However, when the concentration of the solution is too low, the viscosity is correspondingly reduced, and the fibers are easy to settle; too high concentration, larger viscosity, poor fiber dispersion effect and easy occurrence of agglomeration.
S2: weighing boron carbide powder and a mixed solution II according to a mass ratio of 1:5-1:10, and uniformly mixing to obtain a slurry B; the mixed solution II is 0.5-2% of polyacrylamide aqueous solution or hydroxymethyl cellulose sodium aqueous solution; the two dispersing agents are soluble in water, are economical and environment-friendly, and in addition, the aqueous solution with low concentration of the two dispersing agents has higher viscosity, can well disperse powder and is not easy to settle for a long time. However, when the concentration of the solution is too low, the viscosity is correspondingly reduced, and the fibers are easy to settle; too high concentration, larger viscosity, poor fiber dispersion effect and easy occurrence of agglomeration.
S3: mixing the slurry A and the slurry B, and stirring to obtain mixed slurry;
s4: pouring the mixed slurry into a container with a flat bottom surface, placing the container on a vibration table, and vibrating for 10-30 min to uniformly spread the mixed slurry at the bottom of the container;
s5: drying the container in a baking oven at 60-80 deg.C for 4-8 hr, heating to 120-150 deg.C and drying for 2-4 hr to obtain the final product ， The thickness of the sheet is controlled to be 0.5-2mm by controlling the slurry quality per unit area.
Preferably, in step S1, the chopped fiber is one of a carbon fiber, a silicon carbide fiber, and an alumina fiber.
Preferably, in step S1, the length of the chopped fibers is 1 to 6mm.
Preferably, in step S1, the mixing is specifically: the mechanical stirring is carried out by adopting a mixing mode of adding ultrasonic vibration at the same time, the mechanical stirring rotating speed is 600-1000rpm, the ultrasonic vibration frequency is 25-40KHz, and the time is 30-120 min.
Preferably, in step S2, the particle size of the boron carbide powder is 1 to 5 μm.
Preferably, in step S2, the mixing manner specifically includes: the mixing mode of adding ultrasonic vibration while mechanical stirring is adopted, the mechanical stirring rotating speed is 600-1000rpm, the ultrasonic vibration frequency is 25-40KHz, and the time is 30-60 min.
Preferably, in step S3, the stirring speed is 600-1000rpm, and the stirring time is 10-60 min.
Preferably, in the step S4, the vibration time is 10-30 min, the vibration amplitude is 0.5-2mm and the vibration frequency is 10-50 Hz.
In order to achieve the aim, the invention also provides a chopped fiber reinforced boron carbide ceramic sheet, which is prepared by the preparation method.
In order to achieve the above purpose, the invention also provides an application of the chopped fiber reinforced boron carbide ceramic sheet, wherein the boron carbide ceramic sheet prepared by the preparation method or the boron carbide ceramic sheet is applied to the chopped carbon fiber reinforced boron carbide composite material, and can also be combined with a long fiber ceramic sheet to prepare the long and short fiber combined reinforced ceramic matrix composite material.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the chopped fiber reinforced boron carbide ceramic sheet adopts polyacrylamide or sodium hydroxymethyl cellulose as a dispersing agent, chopped fibers and boron carbide powder are respectively and independently dispersed, then dispersion liquid of the chopped fibers and the boron carbide powder is mixed and stirred to form mixed slurry containing the chopped fibers and the boron carbide powder, the mixed slurry is poured into a container with a flat bottom surface, and then the slurry is spread and dried in a vibration mode to obtain the chopped fiber reinforced boron carbide ceramic sheet. The invention adopts a combination mode of mechanical stirring and ultrasonic vibration to solve the problem of uniform dispersion of fibers and powder, the dispersion process has less damage to the fibers, compared with the traditional granulation sieving or ball milling dispersion process of the short fiber reinforced ceramic matrix composite material, the invention maintains the length integrity of the chopped fibers, improves the toughening effect of the fibers in the material, simultaneously, the slurry is rapidly and uniformly spread and dried in a vibration mode, and then the carbon fiber ceramic is prepared into ceramic sheets instead of directly preparing blocks, thereby being beneficial to the preparation of short fiber reinforced boron carbide composite materials with different specifications and sizes, and simultaneously, the invention can also be used in combination with long fiber reinforced boron carbide ceramic sheets or short fiber or long fiber reinforced ceramic sheets of other systems to prepare ceramic matrix composite materials with different composition structures.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a physical view of a chopped fiber reinforced boron carbide ceramic sheet prepared in example 1;
FIG. 2 is a micrograph of a chopped strand fiber reinforced boron carbide ceramic sheet prepared in example 1.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical solutions of the embodiments of the present invention may be combined with each other, but it is necessary to be based on the fact that those skilled in the art can implement the technical solutions, and when the technical solutions are contradictory or cannot be implemented, the combination of the technical solutions should be considered as not existing, and not falling within the scope of protection claimed by the present invention.
The drugs/reagents used are all commercially available without specific description.
Example 1
The embodiment provides a preparation method of a chopped carbon fiber reinforced boron carbide ceramic sheet, which comprises the following steps:
mixing the polyacrylamide solution with the mass fraction of 0.5% with the chopped carbon fibers with the length of 6mm according to the mass ratio of 1:50, and stirring for 30 minutes by adopting a mechanical stirring and ultrasonic vibration mixing mode to obtain the uniformly dispersed fiber slurry A1.
Mixing the polyacrylamide solution with the mass fraction of 0.5% with the boron carbide ceramic powder with the particle size of 1 micrometer according to the mass ratio of 1:10, and stirring for 30 minutes by adopting a mechanical stirring and ultrasonic vibration mixing mode to obtain uniformly dispersed boron carbide slurry B1.
And mixing the slurry A1 and the slurry B1, and further stirring for 60 minutes to obtain uniform slurry containing carbon fibers and boron carbide ceramic powder. Pouring the uniformly dispersed solution into a container with a flat bottom surface, placing the container on a vibration table, vibrating for 10 minutes, and uniformly spreading the slurry at the bottom of the container. After the container is placed in an oven and dried for 4 hours at 60 ℃, the temperature is continuously increased to 150 ℃ and dried for 2 hours, and the chopped carbon fiber reinforced boron carbide ceramic sheet is obtained, the macroscopic and microscopic images of which are shown in figures 1 and 2, and as can be seen from the microscopic images of the chopped carbon fiber reinforced boron carbide ceramic sheet in figure 2, the chopped carbon fiber reinforced silicon carbide ceramic sheet prepared in the embodiment has flat surface and no obvious defects such as fiber aggregation, macroscopic holes and the like, the fibers are uniformly dispersed, and the fiber length is basically undamaged.
Example 2
The embodiment provides a preparation method of a chopped silicon carbide fiber reinforced boron carbide ceramic sheet, which comprises the following steps:
mixing a hydroxymethyl cellulose sodium solution with the mass fraction of 2% with 1mm long and short cut silicon carbide fibers according to the mass ratio of 1:100, and stirring for 120 minutes by adopting a mechanical stirring and ultrasonic vibration mixing mode to obtain uniformly dispersed fiber slurry A2.
Mixing a hydroxymethyl cellulose sodium solution with the mass fraction of 2% with boron carbide ceramic powder with the particle size of 5 microns according to the mass ratio of 1:5, and stirring for 60 minutes by adopting a mechanical stirring and ultrasonic vibration mixing mode to obtain uniformly dispersed boron carbide slurry B2.
And mixing the slurry A2 and the slurry B2, and further stirring for 30 minutes to obtain uniform slurry containing silicon carbide fibers and boron carbide ceramic powder. Pouring the uniformly dispersed solution into a container with a flat bottom surface, placing the container on a vibration table, vibrating for 30 minutes, and uniformly spreading the slurry on the bottom of the container. And (3) placing the container in an oven to dry for 8 hours at 80 ℃, and continuously raising the temperature to 120 ℃ to dry for 4 hours to obtain the chopped silicon carbide fiber reinforced boron carbide ceramic sheet.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the description of the present invention and the accompanying drawings or direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (7)
1. The preparation method of the chopped fiber reinforced boron carbide ceramic sheet is characterized by comprising the following steps of:
s1: weighing chopped fibers and a mixed solution I according to a mass ratio of 1:50-1:100, and uniformly mixing to obtain slurry A; the mixed solution I is a 0.5-2% polyacrylamide solution or a hydroxymethyl cellulose sodium solution; the length of the chopped fiber is 1-6 mm;
s2: weighing boron carbide powder and a mixed solution II according to a mass ratio of 1:2-1:10, and uniformly mixing to obtain a slurry B; the mixed solution II is 0.5-2% of polyacrylamide solution or hydroxymethyl cellulose sodium solution; the grain size of the boron carbide powder is 1-5 microns;
s3: mixing the slurry A and the slurry B, and stirring to obtain mixed slurry;
s4: pouring the mixed slurry into a container with a flat bottom surface, placing the container on a vibration table, and vibrating to uniformly spread the mixed slurry at the bottom of the container;
s5: and (3) placing the container in an oven, drying for 4-8 hours at a low temperature of 60-80 ℃, and continuously heating to 120-150 ℃ and drying for 2-4 hours to obtain the chopped fiber reinforced boron carbide ceramic sheet.
2. The method of claim 1, wherein in step S1, the chopped fiber is one of carbon fiber, silicon carbide fiber, and alumina fiber.
3. The preparation method according to claim 1, wherein in step S1, the mixing is specifically:
the mixing mode of adding ultrasonic vibration while mechanical stirring is adopted, the mechanical stirring rotating speed is controlled at 600-1000rpm, the ultrasonic vibration frequency is 25-40KHz, and the time is 30-120 min.
4. The preparation method according to claim 1, wherein in step S2, the mixing is specifically:
the mixing mode of mechanical stirring and ultrasonic vibration is adopted, the rotating speed is controlled at 600-1000rpm, the frequency of ultrasonic vibration is 25-40KHz, and the time is 30-60 min.
5. The method according to claim 1, wherein in step S3, the stirring speed is 600-1000rpm for 10-60 min.
6. The method according to claim 1, wherein in step S4, the vibration has a frequency of 10-50Hz, an amplitude of 0.5-2mm, and a vibration time of 10-30 min.
7. A chopped fiber reinforced boron carbide ceramic sheet prepared by the preparation method of any one of claims 1 to 6.
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| CN108178647A (en) * | 2017-12-28 | 2018-06-19 | 天津大学 | A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light |
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| WO2003068707A1 (en) * | 2002-02-14 | 2003-08-21 | Toyo Tanso Co., Ltd. | Oxidation resistant carbon fiber reinforced carbon composite material and process for producing the same |
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| CN1600744A (en) * | 2004-10-13 | 2005-03-30 | 中国科学院上海硅酸盐研究所 | Preparation method of enhanced silicon carbide based composite material in short fiber |
| CN101037017A (en) * | 2007-04-29 | 2007-09-19 | 林军 | Vibration material feeding machine of short glass fiber for the screw extruder |
| CN105198304A (en) * | 2015-08-12 | 2015-12-30 | 大连理工大学 | Compound mortar with compound addition of carbon fibers and nano-silica and preparation technology and application thereof |
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| CN108178647A (en) * | 2017-12-28 | 2018-06-19 | 天津大学 | A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light |
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