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CN114644529A - Preparation process of honeycomb-shaped fiber interlayer modern ceramic - Google Patents

Preparation process of honeycomb-shaped fiber interlayer modern ceramic Download PDF

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Publication number
CN114644529A
CN114644529A CN202210441965.9A CN202210441965A CN114644529A CN 114644529 A CN114644529 A CN 114644529A CN 202210441965 A CN202210441965 A CN 202210441965A CN 114644529 A CN114644529 A CN 114644529A
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China
Prior art keywords
ceramic
honeycomb
modern
grain
preparing
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CN202210441965.9A
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Chinese (zh)
Inventor
唐修检
刘谦
谭俊
王帆
吴志远
杜军
王龙
杨理钧
孟凡卓
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Academy of Armored Forces of PLA
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Academy of Armored Forces of PLA
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Priority to CN202210441965.9A priority Critical patent/CN114644529A/en
Publication of CN114644529A publication Critical patent/CN114644529A/en
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Abstract

The invention discloses a preparation process of honeycomb-shaped fiber interlayer modern ceramics, which comprises the following steps: (1) preparing the fine-grain ceramic powder and an adhesive into ceramic slurry, preparing the ceramic slurry into hexagonal prism-shaped solid ceramic cellules, and airing for later use. (2) Preparing interface separating layer slurry by using coarse-grain ceramic powder and an adhesive, wherein the composition of the coarse-grain ceramic powder is consistent with that of the fine-grain ceramic powder, but the size of the coarse-grain ceramic powder is larger than that of the fine-grain ceramic powder; and attaching an interface separation layer on the surface of the ceramic fiber cell body, and drying to obtain a ceramic body. (3) And arranging the ceramic blanks to form a honeycomb structure, then carrying out pressure forming and pressure maintaining to obtain the blanks of the modern ceramic of the self-toughening fiber monolithic. (4) And (4) removing glue from the blank obtained in the step (3), and calcining to obtain the modern ceramic. The ceramic of the invention utilizes the interaction of different structural units to lead cracks to be repeatedly deflected in different structural layers, thereby consuming a great deal of fracture energy and leading the fracture toughness to be increased by geometric multiples.

Description

Preparation process of honeycomb-shaped fiber interlayer modern ceramic
Technical Field
The invention relates to the technical field of modern ceramic preparation, in particular to a preparation process of honeycomb-shaped fiber interlayer modern ceramic.
Background
The modern ceramics have wide application prospect in the fields of aerospace, national defense and military industry, automobiles, mechanical equipment and the like by virtue of excellent performances of corrosion resistance, high temperature resistance, wear resistance, low density and the like. However, the ceramic has the characteristics of high brittleness and low toughness, so that the reliability and the damage resistance of the ceramic are poor, and the further application of the ceramic is limited. The continuous improvement of the toughness of the ceramic has become one of the core problems breaking through the bottleneck of modern ceramic application.
At present, the commonly used ceramic toughening methods include various toughening modes such as phase change toughening, whisker/fiber toughening, microcrack toughening, self toughening, particle toughening, nano toughening, domain transfer, twin toughening and the like. Different toughening modes, toughening principles and application ranges are different. For example, the toughening effect of the particles is not obvious, the toughening cost of the nano particles is high, the large-scale production is difficult, and the like.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation process of honeycomb-shaped fiber interlayer modern ceramics, which has the basic principle that the interaction of different structural units is utilized to lead cracks to be repeatedly deflected in different structural layers, thereby consuming a large amount of fracture energy and increasing the fracture toughness by geometric multiples. In order to achieve the purpose, the invention discloses the following technical scheme:
a preparation process of modern ceramic between honeycomb-shaped fiber layers comprises the following steps:
(1) preparation of ceramic cellule: preparing ceramic slurry from fine-grained ceramic powder and an adhesive, then forming hexagonal prism-shaped solid ceramic cellules from the ceramic slurry by an extrusion method, and airing for later use.
(2) Preparing an interfacial separation layer: preparing interface separating layer slurry from coarse-grain ceramic powder and an adhesive, wherein the composition of the coarse-grain ceramic powder is consistent with that of the fine-grain ceramic powder, but the size of the coarse-grain ceramic powder is larger than that of the fine-grain ceramic powder; and attaching the interface separation layer on the surface of the ceramic cellula body, and drying to obtain a ceramic blank.
(3) And arranging the ceramic blanks to form a honeycomb structure, then carrying out pressure forming and pressure maintaining to obtain the blanks of the modern ceramic of the self-toughening fiber monolithic.
(4) And (4) sintering the green body obtained in the step (3) in a protective atmosphere to remove glue, then continuously calcining in air, and finally performing discharge plasma sintering treatment to obtain the honeycomb-shaped fiber interlayer modern ceramic.
Further, in the step (1), the ceramic powder is made of: b is4C、Al2O3、SiC、TiB2、AlN、Si3N4、ZrO2And the like.
Further, in the step (1), the hexagonal prism-shaped solid ceramic fiber cells are formed by an extrusion method.
Further, in the step (1), the solid content of the ceramic slurry is 40-55%, so that the ceramic celluar body is conveniently prepared.
Further, in the step (1), the diameter of the ceramic fiber cell body is 100-1200 μm.
Further, in the step (1), the ceramic fibrocyte body is dried in the shade for 24-36 hours.
Further, in the steps (1) and (2), the adhesive comprises at least one of polyvinyl alcohol, polyethylene glycol, ethylene glycol and the like. In the invention, the adhesive mainly plays a role in bonding, and can bond ceramic powder together to prepare a ceramic fibroid body.
Further, in the steps (1) and (2), the adhesive is an aqueous solution of the adhesive, so that the ceramic is more uniformly dispersed. Optionally, the mass concentration of the adhesive aqueous solution is 1-5%.
Further, in the step (2), the size of the coarse-grain ceramic powder is at least one order of magnitude larger than that of the fine-grain ceramic powder. Optionally, the grain size of the fine-grain ceramic powder is between 80 nm and 200 nm.
Further, in the step (2), the solid content of the interfacial separation layer slurry is 20-35%. Preferably, the mass ratio of the coarse-grain ceramic powder to the adhesive in the slurry of the interface separation layer is 95-99: 1 to 5.
Further, in the step (2), an interfacial separation layer slurry is attached to the surface of the ceramic fiber cell body by a dipping method to form an interfacial separation layer. Preferably, the thickness of the interfacial separation layer can be controlled by changing the solid content and dipping times of the slurry of the interfacial separation layer.
Further, in the step (2), the drying temperature is 80-90 ℃ and the drying time is 2-3 hours.
Further, in the step (3), the honeycomb ceramic green bodies are arranged in a mold according to one-dimensional orientation, then the honeycomb ceramic green bodies are molded under the pressure of 180-250 MPa, the pressure is maintained for 3-10 min, and the green bodies of the modern ceramic of the self-toughening fiber monoliths are obtained after demolding.
Further, in the step (4), in a protective atmosphere, sintering the obtained blank at 550-700 ℃ for 3-4.5 hours for removing glue, and removing organic matters doped with the ceramic powder. And then preserving heat for 2.5-3.5 hours at 450-550 ℃ in the air to remove the remaining carbide, finally sintering for 5-10 min at 1200-1300 ℃ by adopting a discharge plasma technology, wherein the pressure is 25-30 MPa, and demoulding after the temperature is cooled to room temperature in a cold area to obtain the honeycomb-shaped fiber interlayer modern ceramic.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the ceramic fiber cells of the present invention are arranged in a honeycomb manner, a relatively thin interfacial separation layer is added at each cell interval, and the size of the ceramic crystal grain forming the interfacial separation layer is larger than that of the ceramic fiber cells. The ceramic with the structure has the structural characteristics of dense outside and sparse inside (the outer layer is dense, and the inner layer is gradually loose). The outer layer is compact and can bear larger external pressure; the gradual loosening of the inner layer helps to disperse the borne external pressure into the whole structure, rather than bear the whole external pressure by one point or part of the structure, so that the cracks are repeatedly deflected in different structural layers by utilizing the interaction of different structural units, the fracture energy is consumed greatly, the fracture toughness is increased by geometric multiples, and the brittle nature of the ceramic material is improved to a great extent.
Secondly, the ceramic cellulars are separated by the interface separation layer, so that a plurality of layers are formed while the alternation of soft and hard is realized, and a structure mechanism of soft and hard intersection and multilayer toughening is formed. In addition, the ceramic cellulars and the interface separation layer are made of the same ceramic material, and the grain size of the ceramic of the interface separation layer is larger than that of the ceramic cellulars, so that a ceramic structure with relatively single components is formed through the difference of the grain sizes, therefore, the interface has excellent oxidation resistance under the high-temperature condition while playing a role of inducing the transverse expansion of cracks, the problem that the interface layer is stripped due to thermal mismatch can be avoided, and the stable service under the high-temperature environment for a long time is realized.
Thirdly, the ceramic cellules of the invention are arranged in a honeycomb manner, and the structure has higher stability under compression and shear, thereby reducing the sensitivity of the ceramic to cracks. Meanwhile, the point of the edge intersection of the hexagonal combination of the honeycomb structure is the center of the hexagonal inside, so that the strength of the ceramic is well improved, and the stability of the modern ceramic prepared by the method is further enhanced. In addition, the ceramic of this honeycomb structure has an extremely high degree of adherence. The external forces from the parties can be distributed so that the structure is much more resistant to compressive forces than any round or square shape.
Fourthly, the ceramic fiber cells of the invention are arranged in a honeycomb manner, and the ceramic fiber cells of the invention are arranged in a honeycomb manner, so that the ceramic fiber cells have the characteristic of strong internal independence, and because the relationship between the crack damage of a small-range part and the ceramic fiber cells of other parts in the structure is not large, the ceramic fiber cells of other parts still have good load-bearing capacity.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. The invention will now be further illustrated by specific examples.
Example 1
A preparation process of modern ceramic between honeycomb-shaped fiber layers comprises the following steps:
(1) mixing nano Al2O3Adding the powder (with the particle size of 80-200 nm) into a PVA (polyvinyl alcohol) aqueous solution with the mass concentration of 2%, and uniformly stirring to form Al2O3A slurry having a solids content of 50%. Then adding the Al2O3Extruding the paste to obtain Al with the diameter of 800 mu m2O3And (5) drying the fibroplast in the shade for 24 hours for later use.
(2) Mixing micron Al2O3Dispersing powder (with the particle size of 1-3 microns) in water, adding PVA (polyvinyl alcohol) as a binder, and uniformly stirring to obtain interface separation layer slurry with the solid content of 30%, wherein the micron Al is2O3The mass ratio of the powder to PVA was 99: 1.
(3) Drying the Al2O3Immersing the cellulas into the slurry of the interfacial separation layer in the step (2), taking out the cellulas, and attaching a layer of Al of the slurry of the interfacial separation layer on the surface2O3And drying the fibrocyte body for 3 hours at the temperature of 80 ℃ to obtain a ceramic blank.
(4) And arranging the ceramic blank in a steel die to form a honeycomb structure, then pressurizing to 180MPa for molding, keeping the pressure for 10min by using ice, and demolding to obtain the blank of the modern ceramic of the self-toughening fiber monolithic. Placing the ceramic powder in a tube furnace, keeping the temperature of the ceramic powder at 600 ℃ for 4h in nitrogen for removing glue, and removing PVA in the ceramic powder. Then keeping the temperature in the air at 500 ℃ for 3h to remove the remaining carbide. And finally, sintering for 5min at 1250 ℃ by adopting a discharge plasma sintering technology under the pressure of 25MPa, cooling and demolding after completion to obtain the honeycomb-shaped fiber interlayer modern ceramic.
Example 2
A preparation process of modern ceramic between honeycomb-shaped fiber layers comprises the following steps:
(1) adding nano SiC powder (with the particle size of 80-200 nm) into a PVA (polyvinyl alcohol) aqueous solution with the mass concentration of 2%, and uniformly stirring to form SiC slurry, wherein the solid content of the slurry is 50%. Then, the SiC pulp is extruded out of SiC cellules with the diameter of 100 mu m by an extrusion method, and the SiC cellules are aired in the shade for 30 hours for later use.
(2) Dispersing micron SiC powder (with the particle size of 1-3 microns) in water, adding PVA (polyvinyl alcohol) serving as a binder, and uniformly stirring to obtain interface separation layer slurry with the solid content of 20%, wherein the mass ratio of the micron SiC powder to the PVA is 97: 3.
(3) And (3) immersing the dried SiC cellulose cell body into the interface separation layer slurry in the step (2), taking out the SiC cellulose cell body, and drying the SiC cellulose cell body with the interface separation layer slurry adhered on the surface at 90 ℃ for 2 hours to obtain a ceramic blank.
(4) And arranging the ceramic blank in a steel die to form a honeycomb structure, then pressurizing to 200MPa for molding, keeping the pressure for 5min by using ice, and demolding to obtain the blank of the modern ceramic of the self-toughening fiber monolithic. Placing the ceramic powder in a tube furnace, preserving heat for 4.5 hours at 550 ℃ in nitrogen gas for removing glue, and removing PVA in the ceramic powder. Then keeping the temperature at 450 ℃ in the air for 3.5h to remove the remaining carbide. And finally, sintering for 10min at 1300 ℃ by adopting a discharge plasma sintering technology, wherein the pressure is 30MPa, and cooling and demolding are carried out after the sintering is finished, so that the honeycomb-shaped fiber interlayer modern ceramic is obtained.
Example 3
A preparation process of modern ceramic between honeycomb-shaped fiber layers comprises the following steps:
(1) mixing nano Si3N4Adding the powder (with the particle size of 80-200 nm) into a PVA (polyvinyl alcohol) aqueous solution with the mass concentration of 1%, and uniformly stirring to form Si3N4A slurry having a solids content of 40%. Then the Si is added3N4Extruding Si with the diameter of 300 mu m from the slurry by an extrusion method3N4And drying the cellulosome in the shade for 36 hours for later use.
(2) Mixing micron Si3N4Dispersing powder (with the particle size of 1-3 microns) in water, adding PVA (polyvinyl alcohol) as a binder, and uniformly stirring to obtain interface separation layer slurry with the solid content of 35%, wherein the micron Si is in a size of 1-3 microns3N4The mass ratio of the powder to the PVA was 95: 5.
(3) Drying the dried Si3N4Immersing the cellulum into the interface separating layer slurry in the step (2), taking out the cellulum, and attaching a layer of Si of the interface separating layer slurry on the surface3N4And drying the fibrocyte body for 3 hours at the temperature of 80 ℃ to obtain a ceramic body.
(4) And arranging the ceramic blank in a steel mold to form a honeycomb structure, then pressurizing to 250MPa for molding, keeping the pressure for 3min by using ice, and demolding to obtain the blank of the modern ceramic of the self-toughening fiber monolithic. Placing the ceramic powder in a tube furnace, preserving heat for 3 hours at 700 ℃ in nitrogen gas for glue removal, and removing PVA in the ceramic powder. Then keeping the temperature at 550 ℃ in the air for 2.5h to remove the remaining carbide. And finally, sintering for 10min at 1200 ℃ by adopting a discharge plasma sintering technology, wherein the pressure is 30MPa, and cooling and demolding are carried out after the sintering is finished, so that the honeycomb-shaped fiber interlayer modern ceramic is obtained.
Example 4
A preparation process of modern ceramic between honeycomb-shaped fiber layers comprises the following steps:
(1) nano ZrO is mixed with2Adding the powder (with the particle size of 80-200 nm) into a PVA (polyvinyl alcohol) aqueous solution with the mass concentration of 5%, and uniformly stirring to form ZrO2A slurry having a solids content of 55%. Then the ZrO is oxidized2The slurry is extruded into ZrO with the diameter of 1200 mu m by an extrusion method2And airing the fibrocyte body in a shade for 24 hours for later use.
(2) Forming micro ZrO2Dispersing powder (with the particle size of 1-3 microns) in water, adding PVA (polyvinyl alcohol) as a binder, and uniformly stirring to obtain interface separation layer slurry with the solid content of 30%, wherein the micron ZrO is2The mass ratio of the powder to the PVA was 98: 2.
(3) Subjecting the air-dried ZrO2Immersing the cellullose body into the slurry of the interface separation layer in the step (2), taking out the cellullose body, and attaching a layer of ZrO of the slurry of the interface separation layer on the surface2And drying the fibrocyte body for 2 hours at the temperature of 90 ℃ to obtain a ceramic body.
(4) And arranging the ceramic blank in a steel die to form a honeycomb structure, then pressurizing to 230MPa for molding, keeping the pressure for 4min by using ice, and demolding to obtain the blank of the modern ceramic of the self-toughening fiber monolithic. Placing the ceramic powder in a tube furnace, keeping the temperature of 650 ℃ in nitrogen for 3h for removing glue, and removing PVA in the ceramic powder. Then keeping the temperature in the air at 500 ℃ for 3h to remove the remaining carbide. And finally, sintering for 8min at 1250 ℃ by adopting a discharge plasma sintering technology under the pressure of 25MPa, cooling and demolding after completion to obtain the honeycomb-shaped fiber interlayer modern ceramic.
Example 5
A preparation process of modern ceramic between honeycomb-shaped fiber layers comprises the following steps:
(1) mixing nano Al2O3Adding the powder (with the particle size of 80-200 nm) into a PVA (polyvinyl alcohol) aqueous solution with the mass concentration of 2%, and uniformly stirring to form Al2O3A slurry having a solids content of 50%. Then adding the Al2O3Extruding the paste to obtain Al with the diameter of 800 mu m2O3And (5) drying the fibroplast in the shade for 24 hours for later use.
(2) Drying the Al2O3The fibrocyte body is arranged in a steel mould to form a honeycomb structure, then the pressure is increased by 180MPa for forming, the ice pressure is maintained for 10min, and a blank body of the modern ceramic of the self-toughening fiber monolithic is obtained after demoulding. Placing the ceramic powder in a tube furnace, keeping the temperature of the ceramic powder at 600 ℃ for 4h in nitrogen for removing glue, and removing PVA in the ceramic powder. Then keeping the temperature in the air at 500 ℃ for 3h to remove the remaining carbide. And finally, sintering for 5min at 1250 ℃ by adopting a discharge plasma sintering technology under the pressure of 25MPa, and cooling and demolding after completion to obtain the honeycomb modern ceramic.
Performance testing
The fracture toughness of the ceramics prepared in the above examples was measured, and the results are shown in table 1.
Example number 1 2 3 4 5
Fracture toughness (MPa. m)1/2) 10.6 11.8 10.1 12.3 6.5
Measurement from Table 1As can be seen from the test results, since the interface separation layer and the fibrocyte body are made of the same ceramic material, the crack resistance of the material is improved by inducing cracks to deflect, proliferate, laterally expand and the like by using the coarse-grain interface separation layer, and the fracture toughness of the modern ceramic between the honeycomb-shaped fiber layers prepared in the embodiments 1 to 4 can reach 10 MPa.m1/2The above. Whereas the fracture toughness of the ceramic prepared in example 5 is significantly reduced.
In addition, the stability of the ceramics prepared in the above examples was tested: the results show that after the honeycomb-shaped fiber interlayer modern ceramics prepared in the embodiments 1-4 are subjected to heat treatment for 5 hours at 1000 ℃ in an oxygen environment, the interface layer of the material has no cracking phenomenon, and the retention rate of the fracture toughness can reach over 90%. On the other hand, the ceramic prepared in example 5 exhibited cracking, and the fracture toughness was maintained at 57% or less. The modern ceramic between the honeycomb fiber layers prepared in the embodiments 1-4 can also solve the problem that the heterogeneous interface separation layer is oxidized or the interface layer falls off due to thermal mismatch of a fiber cell body and the interface separation layer, so that the service reliability of the material under a high-temperature condition is improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation process of modern ceramic between honeycomb-shaped fiber layers is characterized by comprising the following steps:
(1) preparation of ceramic cellule: preparing fine-grain ceramic powder and an adhesive into ceramic slurry, then preparing the ceramic slurry into hexagonal prism-shaped solid ceramic cellules, and airing for later use;
(2) preparing an interfacial separation layer: preparing interface separating layer slurry by using coarse-grain ceramic powder and an adhesive, wherein the composition of the coarse-grain ceramic powder is consistent with that of the fine-grain ceramic powder, but the size of the coarse-grain ceramic powder is larger than that of the fine-grain ceramic powder; attaching the interface separation layer on the surface of the ceramic cellula body and then drying to obtain a ceramic blank body;
(3) arranging the ceramic blanks to form a honeycomb structure, then carrying out pressure forming and pressure maintaining to obtain blanks of the modern ceramic of the self-toughening fiber monolithic;
(4) and (4) sintering the green body obtained in the step (3) in a protective atmosphere to remove glue, then continuously calcining in air, and finally performing discharge plasma sintering treatment to obtain the honeycomb-shaped fiber interlayer modern ceramic.
2. The preparation process of the modern ceramic between honeycomb-shaped fiber layers as claimed in claim 1, wherein in step (1), the material of the ceramic powder comprises: b is4C、Al2O3、SiC、TiB2、AlN、Si3N4、ZrO2At least one of (a); preferably, in the step (1), the solid content of the ceramic slurry is 40-55%.
3. The process for preparing modern ceramic between honeycomb-shaped fiber layers in claim 1, wherein in step (1), the hexagonal prism-shaped solid ceramic fiber cells are formed by extrusion.
4. The preparation process of the modern ceramic between honeycomb-shaped fiber layers as claimed in claim 1, wherein in step (1), the diameter of the ceramic fiber cell body is 100-1200 μm; preferably, in the step (1), the ceramic fibrocyte body is dried in the shade for 24-36 hours.
5. The process for preparing the modern ceramic between honeycomb-shaped fiber layers in the claim 1 is characterized in that, in the steps (1) and (2), the adhesive comprises at least one of polyvinyl alcohol, polyethylene glycol and ethylene glycol; preferably, in the steps (1) and (2), the adhesive is an aqueous solution of the adhesive, so that the ceramic is dispersed more uniformly, and preferably, the mass concentration of the aqueous solution of the adhesive is 1-5%.
6. The process for preparing modern ceramic between honeycomb fiber layers as claimed in claim 1, wherein in step (2), the coarse-grained ceramic powder is at least one order of magnitude larger in size than the fine-grained ceramic powder; preferably, the grain size of the fine-grain ceramic powder is 80-200 nm.
7. The process for preparing the modern ceramic between honeycomb-shaped fiber layers as claimed in claim 1, wherein in the step (2), the solid content of the interfacial separation layer slurry is in the range of 20-35%; preferably, the mass ratio of the coarse-grain ceramic powder to the adhesive in the slurry of the interface separation layer is 95-99: 1-5; preferably, in step (2), an interfacial separation layer slurry is attached to the surface of the ceramic fiber cell body by dipping to form an interfacial separation layer.
8. The process for preparing the modern ceramic between honeycomb-shaped fiber layers as claimed in any one of claims 1 to 7, wherein the drying temperature in the step (2) is in the range of 80 to 90 ℃ and the drying time is in the range of 2 to 3 hours.
9. The preparation process of the modern ceramic between honeycomb fiber layers according to any one of claims 1 to 7, characterized in that in step (3), the honeycomb ceramic green bodies are arranged in a mold according to one-dimensional orientation, then are molded under the pressure of 180 to 250MPa, are kept for 3 to 10min, and are demoulded to obtain the green bodies of the modern ceramic of the self-toughening fiber monoliths.
10. The preparation process of the honeycomb-shaped fiber interlayer modern ceramic according to any one of claims 1 to 7, characterized in that in the step (4), the obtained green body is sintered at 550-700 ℃ for 3-4.5 hours in a protective atmosphere to remove glue; then preserving the heat for 2.5 to 3.5 hours at the temperature of 450 to 550 ℃ in the air; and finally, sintering for 5-10 min at 1200-1300 ℃ by adopting a discharge plasma technology, and demoulding after the pressure is 25-30 MPa and the temperature is cooled to room temperature in a cooling zone, thus obtaining the honeycomb-shaped fiber interlayer modern ceramic.
CN202210441965.9A 2022-04-25 2022-04-25 Preparation process of honeycomb-shaped fiber interlayer modern ceramic Pending CN114644529A (en)

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