CN106810286B - Boron nitride fiber reinforced cordierite ceramic matrix composite and preparation method thereof - Google Patents
Boron nitride fiber reinforced cordierite ceramic matrix composite and preparation method thereof Download PDFInfo
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Abstract
A boron nitride fiber reinforced cordierite ceramic matrix composite material and a preparation method thereof. The boron nitride fiber is used as a reinforcing phase, the cordierite powder is used as a raw material, and the ceramic material and the component with specific shapes can be obtained through mixing, molding and sintering. The method comprises the following steps: preparing cordierite powder slurry; pretreating boron nitride fibers; mixing cordierite powder slurry with boron nitride fiber dispersion liquid; removing the solvent; die filling and forming; and hot-pressing and sintering to obtain the boron nitride fiber reinforced cordierite ceramic matrix composite. The boron nitride fiber reinforced cordierite ceramic matrix composite material prepared by the invention has the bending strength of 68-176 MPa and the fracture toughness of 2.2-3.7 MPa.m1/2An elastic modulus of 76 to 143GPa, excellent dielectric properties, and a dielectric constant ε<4.5 dielectric loss tangent value<5.0×10‑3. The high-temperature-resistant wave-transmitting material with good mechanical property can be used for directly preparing special-shaped structural parts with small machining allowance in a large scale.
Description
Technical Field
The invention relates to a boron nitride fiber reinforced cordierite ceramic matrix composite material and a preparation method thereof, belongs to the technical field of heat-proof ceramics, and is particularly suitable for preparing various high-strength heat-proof wave-transparent ceramics.
Background
Cordierite has the chemical formula of Mg2Al4Si5O18Two major crystal forms, high temperature α and low temperature β, high temperature α cordierite has low density and small thermal expansion coefficient (about 2.0 × 10)-6℃-1) Excellent high-temperature stability, good dielectric property and infrared radiation capability, excellent chemical stability and the like, so that the composite material is increasingly applied to the fields of aerospace industry, automobiles, environmental protection, metallurgy, chemical industry, electronic industry and the like with strict requirements on high-temperature resistance and thermal expansion performance.
Cordierite is an important material with a wide application field due to its outstanding properties. Such as acid-corrosion resistant container, hot plate, flame nozzle, ladle pouring nozzle, etc. in chemical and metallurgical industries. In the field of aerospace, the composite material can be used for manufacturing high-technology components such as missile radomes, antenna window cover plates, missile end caps, aerospace plane heat-proof tiles and the like. For example, the antenna cover of beagle dog of the navy of America is made of a material which is developed by corning and takes cordierite as a main crystal phase and is made of 9606 microcrystalline glass. However, pure cordierite ceramics are very limited in practical engineering applications due to their intrinsic brittleness, low strength, low fracture toughness, and susceptibility to stress concentration and microcracking. To improve the mechanical properties of cordierite ceramic materials, fibers are often used as reinforcement to produce composite materials with improved flexural strength and fracture toughness and reduced susceptibility to stress concentration and microcracking. The design and preparation of the fiber reinforced composite material need to consider the physical and chemical differences of the reinforcement and the matrix, such as the thermal expansion coefficients of the reinforcement and the matrix, the crystallization condition at high temperature, the high-temperature stability, the interface reaction and the like. The fibers commonly used at present are mostly continuous fibers, and the fiber materials are mostly carbon or silicon carbide. The mechanical properties of the continuous fibers can be improved to a great extent, but the preparation process is complex, and the components with complex structures are generally difficult to prepare, so that the wide application of the continuous fibers in the engineering field is limited to a great extent. And carbon and silicon carbide fibers have great influence on the dielectric property of the composite material due to the electrical property of the carbon and silicon carbide fibers, so that the application of the carbon and silicon carbide fibers in the field of wave penetration in aerospace is severely limited.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and further provides a boron nitride fiber reinforced cordierite ceramic matrix composite material and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a volume ratio of cordierite powder to boron nitride fiber is A: B, wherein A + B is 100, and B is not less than 5 and not more than 50.
A method for preparing a boron nitride fiber reinforced cordierite ceramic matrix composite,
step one, preparing cordierite powder slurry: placing cordierite powder prepared by a sol-gel method into a ball milling tank, wherein the mass ratio of ball materials is 3-6: 1, adding grinding balls, adding absolute ethyl alcohol into a ball grinding tank, and performing ball milling wet mixing for 6-36 h at a ball milling speed of 30-60 r/min to obtain cordierite powder slurry, wherein the mass fraction of cordierite powder in the cordierite powder slurry is 25-55%;
step two, pretreatment of the boron nitride fiber: shearing the boron nitride fibers with the diameter of 2-10 mu m to obtain boron nitride fibers with the length of 3-5 mm; immersing boron nitride fibers with the length of 3-5 mm into acetone for cleaning for 24-48 h to obtain the boron nitride fibers with the length of 3-5 mm after oil removal and glue removal; dispersing the cleaned boron nitride fibers with the length of 3-5 mm into absolute ethyl alcohol by using the absolute ethyl alcohol as a dispersing agent, and then performing ultrasonic dispersion for 15-30 min under the condition that the ultrasonic power is 200-300W to obtain a boron nitride fiber dispersion liquid;
step three, mixing cordierite powder slurry with boron nitride fiber dispersion liquid: adding the boron nitride fiber dispersion liquid into cordierite powder slurry for 3-6 times, and performing ultrasonic dispersion treatment for 15-30 min under the condition that the ultrasonic power is 200-300W to obtain mixed slurry of cordierite powder and boron nitride fibers;
step four, removing the solvent: stirring the mixed slurry of cordierite powder and boron nitride fiber in an air atmosphere at the temperature of 60-80 ℃ and at the stirring speed of 5-10 r/min, and removing the solvent in the mixed slurry of cordierite powder and boron nitride fiber to obtain a composite blank of cordierite powder and boron nitride fiber;
step five, die filling and forming: loading the cordierite powder and boron nitride fiber composite blank into a graphite die at room temperature, and pre-pressing for 1-3 min under the condition of pre-pressing pressure of 2-5 MPa to obtain the cordierite powder and boron nitride fiber composite blank with a specific shape;
step six, hot-pressing sintering: and heating the pre-pressed cordierite powder and boron nitride fiber composite blank with a specific shape from room temperature to 1000-1400 ℃ under the conditions that the sintering atmosphere is a nitrogen atmosphere, the sintering atmosphere pressure is 0.15-0.25 MPa and the heating rate is 15-30 ℃/min, preserving heat for 15-60 min under the conditions that the sintering atmosphere is a nitrogen atmosphere, the sintering pressure is 10-30 MPa and the sintering temperature is 1000-1400 ℃, and cooling to room temperature along with the furnace after heat preservation is finished to obtain the boron nitride fiber reinforced cordierite composite material.
The invention utilizes the short-cut Boron Nitride (BN) fiber to reinforce the cordierite ceramic, and has the following advantages: 1 BN fiber having a decomposition temperature of 3000 ℃ and excellent dielectric properties, a dielectric constant and a dielectric loss tangent of 3 and 2X 10, respectively-4The material is an ideal high-temperature resistant wave-transmitting material; 2, the preparation forming process is simple, the near net size forming can be realized through model design, and the component can be obtained by non-pressure or hot-pressing sintering, so that the subsequent processing is reduced.
Drawings
Fig. 1 is an XRD diffractogram of the composite material prepared in the first example.
FIG. 2 is a graph of the dielectric constant and the dielectric loss tangent of the composite material prepared in the first example.
FIG. 3 is a fracture morphology plot of the composite prepared in the first example.
As can be seen from the figure, the phase of the composite material consists of α -cordierite and h-BN, and the dielectric constant epsilon is within the frequency band range of 22GHz to 36GHz<4.1 dielectric loss tangent<4.0×10-3The bending strength of the composite material reaches 125MPa, and the fracture toughness is 2.9 MPa.m1/2The elastic modulus is 98GPa, and the elastic modulus is obvious in the fracture processThe fiber can be pulled out, and the strengthening and toughening effects can be effectively achieved.
Detailed Description
The present invention will be described in further detail below: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation is given, but the scope of the present invention is not limited to the following embodiments.
A volume ratio of cordierite powder to boron nitride fiber is A: B, wherein A + B is 100, and B is not less than 5 and not more than 50.
A boron nitride fiber reinforced cordierite ceramic matrix composite material is characterized in that the volume ratio of cordierite powder to boron nitride fiber is 94: 6.
A boron nitride fiber reinforced cordierite ceramic matrix composite material is provided, wherein the volume ratio of cordierite powder to boron nitride fiber is 55: 45.
A preparation method of a boron nitride fiber reinforced cordierite ceramic matrix composite material comprises the following steps:
step one, preparing cordierite powder slurry: placing cordierite powder prepared by a sol-gel method into a ball milling tank, wherein the mass ratio of ball materials is 3-6: 1, adding absolute ethyl alcohol into a ball milling tank, and performing ball milling wet mixing for 6-36 h at a ball milling speed of 30-60 r/min to obtain cordierite powder slurry, wherein the mass fraction of cordierite powder in the cordierite powder slurry is 25-55%.
Step two, pretreatment of the boron nitride fiber: shearing the boron nitride fibers with the diameter of 2-10 mu m to obtain boron nitride fibers with the length of 3-5 mm; immersing boron nitride fibers with the length of 3-5 mm into acetone for cleaning for 24-48 h to obtain the boron nitride fibers with the length of 3-5 mm after oil removal and glue removal; and (3) dispersing the cleaned boron nitride fibers with the length of 3-5 mm into absolute ethyl alcohol by using the absolute ethyl alcohol as a dispersing agent, and then performing ultrasonic dispersion for 15-30 min under the condition that the ultrasonic power is 200-300W to obtain the boron nitride fiber dispersion liquid.
Step three, mixing cordierite powder slurry with boron nitride fiber dispersion liquid: adding the boron nitride fiber dispersion liquid into cordierite powder slurry for 3-6 times, and performing ultrasonic dispersion treatment for 15-30 min under the condition that the ultrasonic power is 200-300W to obtain mixed slurry of cordierite powder and boron nitride fibers.
Step four, removing the solvent: and stirring the mixed slurry of the cordierite powder and the boron nitride fiber in an air atmosphere at the temperature of 60-80 ℃ and at the stirring speed of 5-10 r/min, and removing the solvent in the mixed slurry of the cordierite powder and the boron nitride fiber to obtain the composite blank of the cordierite powder and the boron nitride fiber.
Step five, die filling and forming: and (3) loading the cordierite powder and boron nitride fiber composite blank into a graphite die at room temperature, and pre-pressing for 1-3 min under the condition of pre-pressing pressure of 2-5 MPa to obtain the cordierite powder and boron nitride fiber composite blank with a specific shape.
Step six, hot-pressing sintering: and heating the pre-pressed cordierite powder and boron nitride fiber composite blank with a specific shape from room temperature to 1000-1400 ℃ under the conditions that the sintering atmosphere is a nitrogen atmosphere, the sintering atmosphere pressure is 0.15-0.25 MPa and the heating rate is 15-30 ℃/min, preserving heat for 15-60 min under the conditions that the sintering atmosphere is a nitrogen atmosphere, the sintering pressure is 10-30 MPa and the sintering temperature is 1000-1400 ℃, and cooling to room temperature along with the furnace after heat preservation is finished to obtain the boron nitride fiber reinforced cordierite composite material.
In the first step, the particle size of the cordierite powder is 2.5-5 μm.
In the second step, the boron nitride fiber is hexagonal phase (h-BN).
In the first step, the cordierite powder slurry contains 45% by mass of cordierite powder.
In the first step, wet mixing is carried out for 21 hours under the condition that the ball milling speed is 49 r/min.
In the mixed slurry of the cordierite powder and the boron nitride fiber, the volume ratio of the cordierite powder to the boron nitride fiber is A: B, wherein A + B is 100, and B is not less than 5 and not more than 50.
In the sixth step, the temperature is raised from room temperature to 1360 ℃ under the conditions that the sintering atmosphere is nitrogen atmosphere, the pressure of the sintering atmosphere is 0.19MPa, the temperature raising rate is 22 ℃/min, the sintering pressure is 17MPa, and the sintering temperature is 1380 ℃ and the temperature is kept for 40 min.
Example 1
In the embodiment, a hot-pressing sintering process is adopted, and boron nitride fibers and cordierite powder are taken as raw materials, so that the boron nitride fiber reinforced cordierite ceramic matrix composite material can be obtained;
in the first step, the ball-to-feed ratio is 3:1, the ball-milling rotating speed is 30r/min, the wet mixing time is 24 hours, and the mass fraction of cordierite powder in the cordierite powder slurry is 35%.
In the second step, the diameter of the boron nitride fiber is 6 microns, the length of the boron nitride fiber is 3.5mm, the cleaning time in acetone is 24 hours, the ultrasonic power is 200W, the dispersion time is 20min, and the mass ratio of the boron nitride fiber to the absolute ethyl alcohol is 1: 200.
in the third step, the boron nitride fiber dispersion liquid is added into cordierite powder slurry by 6 times, and then ultrasonic dispersion treatment is carried out for 30min under the ultrasonic power of 200W, and the volume ratio of the cordierite powder to the boron nitride fiber is 70: 30.
In the fourth step, the temperature is 60 ℃, and the stirring speed is 10 r/min.
And step five, pre-pressing at the pressure of 2MPa for 3 min.
In the sixth step, the sintering atmosphere pressure is 0.15MPa, the temperature rise rate is 15 ℃/min, the temperature rises to 1250 ℃, the sintering pressure is 30MPa, and the temperature is kept at 1250 ℃ for 15 min.
The above description is only a preferred embodiment of the present invention, and these embodiments are based on different implementations of the present invention, and the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A preparation method of boron nitride fiber reinforced cordierite ceramic matrix composite material is characterized in that,
step one, preparing cordierite powder slurry: placing cordierite powder prepared by a sol-gel method into a ball milling tank, wherein the mass ratio of ball materials is 3-6: 1, adding grinding balls, adding absolute ethyl alcohol into a ball grinding tank, and performing ball milling wet mixing for 6-36 h at a ball milling speed of 30-60 r/min to obtain cordierite powder slurry, wherein the mass fraction of cordierite powder in the cordierite powder slurry is 25-55%;
step two, pretreatment of the boron nitride fiber: shearing the boron nitride fibers with the diameter of 2-10 mu m to obtain boron nitride fibers with the length of 3-5 mm; immersing boron nitride fibers with the length of 3-5 mm into acetone for cleaning for 24-48 h to obtain the boron nitride fibers with the length of 3-5 mm after oil removal and glue removal; dispersing the cleaned boron nitride fibers with the length of 3-5 mm into absolute ethyl alcohol by using the absolute ethyl alcohol as a dispersing agent, and then performing ultrasonic dispersion for 15-30 min under the condition that the ultrasonic power is 200-300W to obtain a boron nitride fiber dispersion liquid;
step three, mixing cordierite powder slurry with boron nitride fiber dispersion liquid: adding the boron nitride fiber dispersion liquid into cordierite powder slurry for 3-6 times, and performing ultrasonic dispersion treatment for 15-30 min under the condition that the ultrasonic power is 200-300W to obtain mixed slurry of cordierite powder and boron nitride fibers;
step four, removing the solvent: stirring the mixed slurry of cordierite powder and boron nitride fiber in an air atmosphere at the temperature of 60-80 ℃ and at the stirring speed of 5-10 r/min, and removing the solvent in the mixed slurry of cordierite powder and boron nitride fiber to obtain a composite blank of cordierite powder and boron nitride fiber;
step five, die filling and forming: loading the cordierite powder and boron nitride fiber composite blank into a graphite die at room temperature, and pre-pressing for 1-3 min under the condition of pre-pressing pressure of 2-5 MPa to obtain the cordierite powder and boron nitride fiber composite blank with a specific shape;
step six, hot-pressing sintering: and heating the pre-pressed cordierite powder and boron nitride fiber composite blank with a specific shape from room temperature to 1000-1400 ℃ under the conditions that the sintering atmosphere is a nitrogen atmosphere, the sintering atmosphere pressure is 0.15-0.25 MPa and the heating rate is 15-30 ℃/min, preserving heat for 15-60 min under the conditions that the sintering atmosphere is a nitrogen atmosphere, the sintering pressure is 10-30 MPa and the sintering temperature is 1000-1400 ℃, and cooling to room temperature along with the furnace after heat preservation is finished to obtain the boron nitride fiber reinforced cordierite composite material.
2. The method for preparing the boron nitride fiber reinforced cordierite ceramic matrix composite material according to claim 1, wherein the particle size of the cordierite powder in the first step is 2.5-5 μm.
3. The method according to claim 1, wherein the boron nitride fibers in step two are hexagonal phase (h-BN).
4. The method according to claim 1, wherein the cordierite powder slurry of step one contains 45% by mass of cordierite powder.
5. The method according to claim 1, wherein in the first step, the wet mixing is performed at a ball milling speed of 49r/min for 21 hours.
6. The method according to claim 1, wherein in the slurry mixture of cordierite powder and boron nitride fiber in step three, the volume ratio of cordierite powder to boron nitride fiber is A: B, wherein A + B is 100, and B is 5. ltoreq. B.ltoreq.50.
7. The method according to claim 1, wherein in step six, the sintering atmosphere is nitrogen, the temperature is raised from room temperature to 1360 ℃ under the conditions that the pressure of the sintering atmosphere is 0.19MPa and the temperature raising rate is 22 ℃/min, the sintering pressure is 17MPa, and the sintering temperature is 1380 ℃ and the temperature is kept for 40 min.
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| CN108823513A (en) * | 2018-07-19 | 2018-11-16 | 合肥连森裕腾新材料科技开发有限公司 | A kind of preparation process of the metal matrix ceramic composites of doping composite fiber |
| CN109053169A (en) * | 2018-07-27 | 2018-12-21 | 哈尔滨工业大学 | A kind of densification boron nitride crystal whisker enhancing vitreous silica composite ceramics and preparation method |
| CN110066176A (en) * | 2019-05-13 | 2019-07-30 | 山东理工大学 | The preparation method of boron nitride fiber enhancing silicon boron oxygen nitrogen ceramic matric composite |
| CN113233773B (en) * | 2021-04-28 | 2023-06-16 | 中国电子科技集团公司第四十三研究所 | LTCC substrate material and preparation method thereof |
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| CN115385705B (en) * | 2022-09-30 | 2023-08-18 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber mat and preparation method thereof |
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