CN114477950B - Preparation method of ceramic matrix composite based on aramid fiber fabric - Google Patents
Preparation method of ceramic matrix composite based on aramid fiber fabric Download PDFInfo
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- CN114477950B CN114477950B CN202210262344.4A CN202210262344A CN114477950B CN 114477950 B CN114477950 B CN 114477950B CN 202210262344 A CN202210262344 A CN 202210262344A CN 114477950 B CN114477950 B CN 114477950B
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/08—Impregnating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/20—All layers being fibrous or filamentary
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/51—Elastic
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
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- C04B2111/00379—Materials containing oriented fillers or elements the oriented elements being fibres
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Abstract
The invention discloses a preparation method of a ceramic matrix composite based on aramid fiber fabric, which comprises the following steps:S1adding water, bentonite and sodium polyacrylate into light calcium carbonate, and uniformly mixing to prepare calcium carbonate ceramic slurry; s2, placing the aramid fiber fabric into a muffle furnace for low-temperature oxidation to remove the organic binder, preserving heat at an oxidation temperature, soaking the pre-oxidized aramid fiber fabric into a dilute nitric acid/acetone solution, repeatedly washing the pre-oxidized aramid fiber fabric with deionized water until the solution is neutral, and uniformly cutting the pre-oxidized aramid fiber fabric into aramid fiber fabric wafers; and S3, putting the pretreated aramid fiber fabric wafer and the calcium carbonate ceramic slurry into an ultrasonic instrument. And S4, stacking the impregnated aramid fiber fabrics in a cold-burning mold, preserving the heat for a period of time at a certain temperature and under a certain pressure, and drying the aramid fiber fabrics. The tensile strength and the elastic modulus of the fiber fabric are enhanced, the preparation method is simple, the temperature is lower, the safety is higher, and the cost is greatly reduced.
Description
Technical Field
The invention belongs to the field of protective materials and preparation and application thereof, and particularly relates to a preparation method of a ceramic matrix composite based on aramid fiber fabric.
Background
Aramid fibers begin to decompose at temperatures in excess of 370 c and begin to carbonize at around 400 c, and ceramic slurry and fibers cannot be bonded by the previous high temperature sintering methods. In 2016, the Clive Randall professor of the university of Pennsylvania State university in Material science and engineering and his colleagues developed a new technology called the Cold Sintering Process (CSP-Cold Sintering Process), which requires only 200 ℃ at the maximum to produce ceramics and can complete Sintering within 15 minutes at the minimum, thus greatly reducing the cost of industrial manufacture. Meanwhile, the technology also improves the binding capacity of originally incompatible materials (such as ceramics and plastics), and provides possibility for creating more useful novel composite materials.
Therefore, the invention provides a preparation method of a ceramic matrix composite based on aramid fiber fabric by combining a cold burning process with the function of ceramic reinforced fiber.
Disclosure of Invention
A preparation method of a ceramic matrix composite based on aramid fiber fabric comprises the following steps:
s1, adding water, bentonite and sodium polyacrylate into light calcium carbonate, and uniformly mixing to prepare calcium carbonate ceramic slurry;
s2, placing the aramid fiber fabric into a muffle furnace for low-temperature oxidation to remove organic binders on the fiber surface, preserving heat at a certain oxidation temperature, soaking the pre-oxidized aramid fiber fabric into a dilute nitric acid/acetone solution, adjusting functional groups on the fiber surface, repeatedly washing the aramid fiber fabric with deionized water until the solution is neutral, and uniformly cutting the pre-treated aramid fiber fabric into aramid fiber fabric wafers with the same specification as that of a cold-burning mold;
s3, placing the aramid fiber fabric wafer pretreated in the step S2 and the calcium carbonate ceramic slurry prefabricated in the step S1 into an ultrasonic instrument, and exhausting air through a conduit connected with a vacuum pump;
and S4, stacking the aramid fiber fabrics impregnated in the step S3 into a cold-burning mold, preserving heat for a period of time at a certain temperature and under a certain pressure, and drying to obtain the target material.
Preferably, the mass ratio of the light calcium carbonate, the water, the bentonite and the sodium polyacrylate in the step S1 is 10.
Preferably, the oxidation temperature in the step S2 is 300-310 ℃, and the heat preservation time is 3-4 min.
Preferably, the soaking time in the step S2 is 23-24 h.
Preferably, the ultrasonic time in the step S3 is 2h-2.5h, and the ultrasonic temperature is 60-80 ℃.
Preferably, in the step S4, the temperature is 190-200 ℃, the pressure is 500-550 MPa, and the heat preservation time is 30-35 min.
Preferably, the number of the stacking layers of the aramid fiber fabrics impregnated in the step S4 is 5 to 10.
The invention has the beneficial effects that:
on the basis of not damaging the aramid fiber fabric, the calcium carbonate ceramic is dipped into the aramid fiber fabric for cold sintering, so that the tensile strength and the elastic modulus of the fiber fabric are enhanced. Meanwhile, the preparation method of the material is simple, the production temperature is low, the material is safer, and the production cost is greatly reduced compared with the traditional high-temperature sintering.
Drawings
FIG. 1 is a line graph showing the bending strength of samples 1, 2, 3 and 4 obtained in example 1, 2, 1 and 2;
FIG. 2 is a line graph showing the elastic modulus of samples 1, 2, 3 and 4 obtained in example 1, 2, 1 and 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Example 1
A preparation method of a ceramic matrix composite based on aramid fiber fabric comprises the following steps:
s1, adding water, bentonite and sodium polyacrylate into light calcium carbonate in a mass ratio of 10
Evenly mixing to prepare calcium carbonate ceramic slurry;
s2, placing the aramid fiber fabric into a muffle furnace for low-temperature oxidation to remove the organic binder on the surface of the fiber, and preserving heat at 300 ℃; soaking the pre-oxidized aramid fiber fabric in a dilute nitric acid/acetone solution for 24 hours, adjusting functional groups on the surface of the fiber, repeatedly washing the aramid fiber fabric with deionized water until the solution is neutral, and uniformly cutting the pre-treated aramid fiber fabric into aramid fiber fabric wafers with the same specification as that of a cold-fired mold;
s3, placing the aramid fiber fabric wafer pretreated in the step S2 and the calcium carbonate ceramic slurry prefabricated in the step S1 into an ultrasonic instrument, wherein the ultrasonic time is 2.5 hours, the ultrasonic temperature is 80 ℃, and extracting air by connecting a vacuum pump guide pipe;
and S4, placing the 6 layers of the aramid fiber fabric dipped in the step S3 in a cold-burning mould, preserving heat for 35min at 200 ℃ and 550MPa, and drying to obtain a sample 1. Through detection, the bending strength of the sample 1 reaches 600MPa, and the elastic modulus reaches 360GPa.
Example 2
Wherein the steps S1-S2 are the same as in example 1;
s3, placing the aramid fiber fabric wafer pretreated in the step S2 and the prefabricated calcium carbonate ceramic slurry prepared in the step S1 into an ultrasonic instrument, carrying out ultrasonic treatment for 2 hours at the ultrasonic temperature of 60 ℃, and extracting air by connecting a vacuum pump guide pipe;
and S4, placing the laminated 6 layers of the aramid fiber fabric dipped in the step S3 into a cold-burning mold, preserving the heat for 30min at 200 ℃ and 500MPa, and drying the aramid fiber fabric to obtain a sample 2. Through detection, the bending strength of the sample 2 reaches 580MPa, and the elastic modulus reaches 325GPa.
Comparative example 1
Wherein the steps S1 to S3 are the same as in example 1;
and S4, placing the laminated 6 layers of the aramid fiber fabric dipped in the step S3 into a cold-burning mold, preserving the heat for 30min at 150 ℃ and 400MPa, and drying the aramid fiber fabric to obtain a sample 3. The test shows that the bending strength of the sample 3 only reaches 400MPa, and the elastic modulus reaches 310GPa.
Comparative example 2
Wherein the steps S1 to S3 are the same as in example 1;
and S4, placing the 6 layers of the aramid fiber fabric layer dipped in the step S3 into a cold-burning mould, preserving the heat for 30min at 180 ℃ and 500MPa, and drying to obtain a sample 4. The bending strength of the sample 4 is only 420MPa, and the elastic modulus is 320GPa.
It should be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (5)
1. A preparation method of a ceramic matrix composite based on aramid fiber fabric is characterized by comprising the following steps:
s1, preparing calcium carbonate ceramic slurry:
adding water, bentonite and sodium polyacrylate into light calcium carbonate, and uniformly mixing to prepare calcium carbonate ceramic slurry, wherein the mass ratio of the light calcium carbonate to the water to the bentonite to the sodium polyacrylate is (10);
s2, pretreating aramid fiber fabric:
placing the aramid fiber fabric into a muffle furnace for low-temperature oxidation to remove organic binders on the fiber surface, preserving heat at a certain oxidation temperature, soaking the pre-oxidized aramid fiber fabric into a dilute nitric acid/acetone solution, adjusting functional groups on the fiber surface, repeatedly washing the aramid fiber fabric with deionized water until the solution is neutral, and uniformly cutting the pre-treated aramid fiber fabric into aramid fiber fabric wafers with the same specification as that of a cold-fired mold;
s3, slurry impregnation:
putting the aramid fiber fabric wafer pretreated in the step S2 and the calcium carbonate ceramic slurry prefabricated in the step S1 into an ultrasonic instrument, and extracting air by connecting a vacuum pump guide pipe;
s4, cold sintering:
and (4) stacking the aramid fiber fabrics impregnated in the step (S3) into a cold-burning mould, preserving the heat for 30-35 min at the temperature of 190-200 ℃ and under the pressure of 500-550 MPa, and drying to obtain the target material.
2. The preparation method of the ceramic matrix composite based on the aramid fiber fabric according to claim 1, wherein the oxidation temperature in the step S2 is 300-310 ℃, and the heat preservation time is 3-4 min.
3. The method for preparing the ceramic matrix composite based on the aramid fiber fabric according to the claim 1, wherein the soaking time in the step S2 is 23-24 h.
4. The method for preparing the ceramic matrix composite based on the aramid fiber fabric according to claim 1, wherein the ultrasonic time in the step S3 is 2h-2.5h, and the ultrasonic temperature is 60-80 ℃.
5. The method for preparing the ceramic matrix composite based on the aramid fiber fabric according to the claim 1, wherein the number of the stacking layers of the aramid fiber fabric impregnated in the step S4 is 5-10.
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| CN202210262344.4A CN114477950B (en) | 2022-03-17 | 2022-03-17 | Preparation method of ceramic matrix composite based on aramid fiber fabric |
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| CN114477950B true CN114477950B (en) | 2022-10-18 |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4365152A2 (en) * | 2015-09-29 | 2024-05-08 | The Penn State Research Foundation | Cold sintering ceramics and composites |
| US10730803B2 (en) * | 2015-09-29 | 2020-08-04 | The Penn State Research Foundation | Cold sintering ceramics and composites |
| TW201825438A (en) * | 2016-08-26 | 2018-07-16 | 美商薩比克環球應用科技公司 | Ceramic composite devices and methods |
| CN108821788A (en) * | 2018-07-24 | 2018-11-16 | 合肥岑遥新材料科技有限公司 | A kind of corrosion resistant ceramic matric composite and preparation method thereof |
| CN110372998B (en) * | 2019-07-30 | 2020-07-07 | 山东大学 | Aramid fiber reinforced epoxy resin matrix composite material and preparation method thereof |
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