CN116354736A - Preparation method of fiber reinforced alumina ceramic matrix composite - Google Patents
Preparation method of fiber reinforced alumina ceramic matrix composite Download PDFInfo
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- CN116354736A CN116354736A CN202310307710.8A CN202310307710A CN116354736A CN 116354736 A CN116354736 A CN 116354736A CN 202310307710 A CN202310307710 A CN 202310307710A CN 116354736 A CN116354736 A CN 116354736A
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- 239000000835 fiber Substances 0.000 title claims abstract description 188
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000005336 cracking Methods 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001723 curing Methods 0.000 claims abstract description 14
- 238000007598 dipping method Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000011265 semifinished product Substances 0.000 claims abstract description 6
- 230000004584 weight gain Effects 0.000 claims abstract description 6
- 235000019786 weight gain Nutrition 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 4
- 239000004744 fabric Substances 0.000 claims description 36
- 238000009958 sewing Methods 0.000 claims description 30
- 238000005470 impregnation Methods 0.000 claims description 23
- 238000004321 preservation Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 40
- 239000000463 material Substances 0.000 abstract description 31
- 230000014759 maintenance of location Effects 0.000 abstract description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 31
- 238000000197 pyrolysis Methods 0.000 description 25
- 230000008569 process Effects 0.000 description 20
- 239000011159 matrix material Substances 0.000 description 15
- 238000005452 bending Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 238000013001 point bending Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 230000003685 thermal hair damage Effects 0.000 description 4
- 239000011184 SiC–SiC matrix composite Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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Abstract
A preparation method of a fiber reinforced alumina ceramic matrix composite material is provided, which comprises the following steps: s1, performing high-temperature heat treatment on a fiber prefabricated member to obtain a fiber prefabricated member to be impregnated; s2, dipping, drying and solidifying the fiber prefabricated member to be dipped by adopting silica sol to obtain a fiber prefabricated member with a silica interface layer; s3, adopting an alumina precursor solution to impregnate, dry and solidify and crack a fiber preform with a silica interface layer at high temperature to obtain a fiber reinforced alumina ceramic matrix composite semi-finished product; s4, carrying out dipping, drying, curing and high-temperature cracking on the semi-finished product of the fiber reinforced alumina ceramic matrix composite for a plurality of times until the weight gain rate of the weight of the fiber reinforced alumina ceramic matrix composite is lower than a preset value compared with the weight gain rate of the fiber reinforced alumina ceramic matrix composite after the previous high-temperature cracking, thus obtaining the finished product of the fiber reinforced alumina ceramic matrix composite. The strength retention rate of the composite material prepared by the method is higher than 80% after the high-temperature heat treatment at 1400 ℃ for 1 h.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method of a fiber reinforced alumina ceramic matrix composite material.
Background
Continuous alumina fiber reinforced alumina ceramic matrix composite (Al 2 O 3f /Al 2 O 3 ) The material is a material compounded by taking continuous alumina fiber as a reinforcement body and alumina ceramic as a matrix, and the components of the material system are all oxides, compared with metal materials such as titanium alloy, high-temperature alloy and the like, al 2 O 3f /Al 2 O 3 The composite material has higher temperature resistance (the long-term use temperature can reach 1200 ℃), and lower density (about 1/3 of the superalloy); compared with SiC/SiC composite material, al 2 O 3f /Al 2 O 3 The composite material has better oxidation resistance and lower cost (about 1/3 of that of the SiC/SiC composite material), and Al 2 O 3f /Al 2 O 3 The composite material has obvious cost advantage compared with a potential aerospace vehicle high-temperature component candidate material SiC/SiC composite material, and has obvious weight reduction advantage compared with the existing common material superalloy of the aerospace vehicle high-temperature component.
The prepreg-hot press sintering process is Al which is realized and applied at present 2 O 3f /Al 2 O 3 The most commonly adopted process of the composite material is that after the fiber is soaked into ceramic slurry to prepare prepreg, the prepreg is formed into a composite material blank of fiber/matrix through layering or winding, and Al is obtained after hot-pressing sintering 2 O 3f /Al 2 O 3 A composite material. The process has the advantages that: (1) The surface of the fiber does not need to prepare an interface layer, the fiber does not need to be subjected to three-dimensional braiding treatment, and the subsequent repeated dipping-cracking process is not needed, so that the loss of the preparation process on the fiber performance can be reduced; (2) The prepreg-hot pressing sintering process has simple procedures, so that the preparation efficiency is higher, and the production and the application of the prepreg-hot pressing sintering process are facilitated.
Meanwhile, the prepreg-hot pressing sintering process generally needs to be prepared at a temperature of more than 1000 ℃, so that great thermal damage is caused to the fibers, and high-temperature diffusion reaction between the fibers and a matrix is easily caused to form strong interface bonding. The hot press sintering process has high requirements on equipment and is not suitable for being used as a component with a complex shape.
In China Al 2 O 3f /Al 2 O 3 Composite materials are studied at the beginning stage, and the composite material performance is generally low, and the root cause is that the fiber performance is greatly reduced due to the fact that the sintering temperature of a composite material matrix is too high.
Thus, a process has been developed which can produce Al at relatively low temperatures 2 O 3f /Al 2 O 3 The composite material is beneficial to obtaining more excellent performance.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a preparation method of a fiber reinforced alumina ceramic matrix composite. The preparation method of the invention avoids the formation of strong interface bonding, and has short period and simple and convenient process.
The technical scheme of the invention is that the preparation method of the fiber reinforced alumina ceramic matrix composite material comprises the following steps:
s1, performing high-temperature heat treatment on a fiber prefabricated member to obtain a fiber prefabricated member to be impregnated;
s2, dipping, drying and solidifying the fiber prefabricated member to be dipped by adopting silica sol to obtain a fiber prefabricated member with a silica interface layer;
s3, adopting an alumina precursor solution to impregnate, dry and solidify and crack a fiber preform with a silica interface layer at high temperature to obtain a fiber reinforced alumina ceramic matrix composite semi-finished product;
s4, carrying out dipping, drying, curing and high-temperature cracking on the semi-finished product of the fiber reinforced alumina ceramic matrix composite for 5-10 times until the weight gain rate of the weight of the fiber reinforced alumina ceramic matrix composite is lower than a preset value compared with the weight gain rate of the fiber reinforced alumina ceramic matrix composite after the previous high-temperature cracking, thus obtaining the finished product of the fiber reinforced alumina ceramic matrix composite.
Further, before step S1, the method further includes:
cutting the alumina fiber cloth according to the required size;
disassembling the alumina fiber cloth to obtain a required suture line;
and sewing the cut alumina fiber cloth by adopting a suture line to obtain a fiber prefabricated member.
Further, the above-mentioned sewing mode is double-thread sewing, and the sewing interval is 3mm×3mm to 15mm×15mm
Further, in the step S1, the high-temperature heat treatment conditions are as follows: the temperature is 500-800 ℃, the inert atmosphere is used, and the heat preservation time is 0.5-2 h.
Further, in the steps S2 to S4, the impregnation mode is vacuum impregnation, the pressure is reduced to-0.1 MPa, and the impregnation time is 2 to 8 hours.
Further, in the steps S2 to S4, the curing temperature is 150 ℃ to 200 ℃ and the heat preservation time is 2 hours to 8 hours.
Further, in the steps S3 to S4, the high-temperature cracking temperature is 700 ℃ to 900 ℃, the heat preservation time is 0.5h to 2h, and the cracking atmosphere is air or inert atmosphere.
Further, in the step S4, the preset value is 1wt%.
Compared with the prior art, the invention has the advantages that:
1. compared with the prior art, the density of the composite material prepared by the invention is 2.06g/cm 3 ～2.13g/cm 3 The porosity is 10% -15%, the bending strength is 150-180 MPa at room temperature, and the strength retention rate is higher than 80% after the high-temperature heat treatment for 1h at 1400 ℃.
2. It has been found that some form of chemical reaction between the precursor and the fibers occurs during the pyrolysis process or that the elements in the precursor diffuse into the fibers under the high temperature of the pyrolysis process. The reaction and diffusion results are: on one hand, the fiber is seriously damaged, the fiber strength is greatly reduced, the material strength is not high, and on the other hand, a strong-bonding interface layer is formed, the fiber toughening effect is poor, and the material toughness is low.
1) When the interface layer is prepared, only one round of dipping-curing is carried out, and high-temperature cracking is not carried out, so that the thermal damage and mechanical damage of the fiber can be reduced, the condition that the fiber is strongly combined with the interface layer is avoided, and the toughening effect of the fiber is ensured; thermal damage includes, among other things, thermal physical damage to the fibers at high temperatures, and thermal stress damage to the fibers and interface layers due to thermal expansion mismatch.
2) The oxide organic precursor is adopted as an interface layer, and no reaction occurs with the fiber, so that the performance degradation of the alumina fiber is avoided; in addition, the oxide organic precursor is used as a raw material to prepare the silica interface layer, so that the wettability of the precursor and the fiber is increased.
3) And only one round of dipping-curing is carried out, the organic solvent in the silica sol is removed, so that a silica interface layer is obtained, the interface layer can be ensured not to react before the composite material is subjected to high-temperature densification cracking, so that a weak interface is formed between the fiber and the matrix, and finally, the reinforcing and toughening effects of the composite material are realized. The toughening mechanism for finally obtaining the weak interface phase in the scheme is as follows: when the composite material bears an external load and cracks are expanded to a weak interface phase, crack deflection can occur at the interface along the fiber axial direction, and then the crack deflection continues to expand along the fiber axial direction, so that the fracture energy is consumed, and the strength and toughness of the material are improved.
4) The invention considers that the interface layer is cracked at the same time when the subsequent sintering (high-temperature cracking) of the ceramic matrix is carried out, and the invention is equivalent to retarding the high-temperature cracking of the interface layer to be carried out simultaneously with the ceramic matrix, and controls the interface bonding strength through the repeated times of the alumina precursor dipping-curing-high-temperature cracking in the stage of the ceramic matrix, so that the material densification efficiency can be improved without carrying out the high-temperature cracking when the interface layer is prepared, the densification times are reduced, namely, the preparation flow is shortened, and the process is simplified.
3. The invention adopts the organic-inorganic conversion method to prepare the composite material, has simple steps and low requirements on environment and equipment, can effectively prepare complex special-shaped components, and is suitable for batch production of the composite material; the cracking temperature of the organic-inorganic conversion method is not higher than 900 ℃, so that the thermal damage to the fiber is effectively reduced, the strength of the reinforcement fiber is maintained, and the strength of the composite material is improved.
4. The invention has flexible structural design on the composite material, realizes the structural control of the composite material by impregnating the precursor liquid, and meets different use requirements.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a schematic flow chart of a method for preparing a fiber reinforced alumina ceramic matrix composite in an embodiment of the invention;
FIG. 2 shows Al in the embodiment of the invention 2 O 3f /Al 2 O 3 A preparation process flow chart of the composite material;
FIG. 3 shows the Al prepared in example 1 of the present invention 2 O 3f /Al 2 O 3 SEM image of the composite.
FIG. 4 shows Al prepared in example 3 and comparative example 3 of the present invention 2 O 3f /Al 2 O 3 Load displacement curve graph of composite material;
FIG. 5 shows the Al prepared in comparative example 1 of the present invention 2 O 3f /Al 2 O 3 SEM image of the composite.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and detailed description for the purpose of enabling those skilled in the art to understand the invention better.
As shown in fig. 1, a schematic flow chart of a method of preparing a fiber reinforced alumina ceramic matrix composite is provided.
Example 1
A preparation method of a vitamin-reinforced alumina ceramic matrix composite material comprises the following preparation processes:
(1) First, al is mixed with 2 O 3 The fiber cloth was cut to a size of 100mm×70mm×0.33mm (length×width×height), and the fiber cloth was disassembled to obtain a desired suture. Al (Al) 2 O 3 And (3) superposing every 9 pieces of fiber cloth (aligning the edges of the fiber cloth as much as possible), and sewing the fiber cloth by adopting the obtained sewing line, wherein the sewing mode is double-line sewing, the sewing interval is 5mm multiplied by 5mm, and the fiber prefabricated member with the thickness of 3mm is obtained.
(2) The fiber prefabricated member is put into a muffle furnace for pretreatment, the impregnating compound on the surface of the fiber is removed, and the pretreatment conditions are as follows: inert atmosphere at 500 ℃ for 50min, and then cooling to room temperature along with the furnace to finish pretreatment.
(3) And placing the pretreated fiber prefabricated member into a vacuum impregnation tank, and vacuumizing until the pressure is reduced to-0.1 MPa. Introducing silica sol into an impregnation tank, and impregnating the fiber preform for 2 hours; and (3) putting the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 150 ℃, and continuously baking for 8 hours.
(4) Will complete SiO 2 The sol impregnated-solidified fiber preform is placed in a vacuum impregnation tank and vacuumized until the pressure is reduced to-0.1 MPa. Al is added with 2 O 3 The precursor solution is led into an impregnating tank to impregnate the fiber prefabricated member, and the impregnating time is 2 hours; placing the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 150 ℃, and continuously baking for 8 hours; will finish Al 2 O 3 Placing the sol impregnated-solidified fiber preform into a muffle furnace for high-temperature pyrolysis, wherein the pyrolysis temperature is 900 ℃, the pyrolysis time is 1h, and the pyrolysis atmosphere is air atmosphere, so as to initially obtain the fiber reinforced alumina ceramic matrix composite material with lower density; repeating the dipping, curing and cracking for 5 times to obtain compact Al 2 O 3f /Al 2 O 3 A composite material.
Al prepared in this example 2 O 3f /Al 2 O 3 The open porosity of the composite material is 12.5% and the density is 2.06g/cm measured by Archimedes drainage method 3 . The SEM photograph of fig. 3 clearly shows the interface between the fibers/matrix thereof, indicating that the interfacial reaction between the fibers and the matrix is effectively avoided by the present method. The bending strength at room temperature is 178MPa by a three-point bending test, and a typical ductile fracture mode is shown. After high temperature heat treatment at 1400 ℃ for 1h, the bending strength is 148MPa, and the strength retention rate is 83.1%.
Example 2
The preparation method of the fiber reinforced alumina ceramic matrix composite material comprises the following preparation processes:
(1) First, al is mixed with 2 O 3 The fiber cloth was cut to a size of 150mm×100mm×0.33mm (length×width×height), and the fiber cloth was disassembled to obtain a desired suture. Al (Al) 2 O 3 The fiber cloth is overlapped in a group of every 10 pieces (the edges of the fiber cloth are aligned as much as possible), and the fiber cloth is sewn by adopting the obtained sewing thread, wherein the sewing mode is double-thread sewing, the sewing interval is 10mm multiplied by 10mm, and the fiber prefabricated member with the thickness of 3mm is obtained.
(2) The fiber prefabricated member is put into a muffle furnace for pretreatment, the impregnating compound on the surface of the fiber is removed, and the pretreatment conditions are as follows: inert atmosphere at 800 ℃ for 30min, and then cooling to room temperature along with the furnace to finish pretreatment.
(3) And placing the pretreated fiber prefabricated member into a vacuum impregnation tank, and vacuumizing until the pressure is reduced to-0.1 MPa. Introducing silica sol into an impregnation tank, and impregnating the fiber preform for 2 hours; and (3) putting the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 200 ℃, and continuously baking for 2 hours.
(4) Will complete SiO 2 The sol impregnated-solidified fiber preform is placed in a vacuum impregnation tank and vacuumized until the pressure is reduced to-0.1 MPa. Al is added with 2 O 3 The precursor solution is led into an impregnating tank to impregnate the fiber prefabricated member, and the impregnating time is 2 hours; placing the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 200 ℃, and continuously baking for 2 hours; will finish Al 2 O 3 Placing the sol impregnated-solidified fiber preform into a muffle furnace for high-temperature pyrolysis, wherein the pyrolysis temperature is 700 ℃, the pyrolysis time is 2 hours, and the pyrolysis atmosphere is air atmosphere, so as to obtain the fiber reinforced alumina ceramic matrix composite material with lower density preliminarily; repeating the dipping, curing and cracking for 7 times to obtain compact Al 2 O 3f /Al 2 O 3 A composite material.
Al prepared in this example 2 O 3f /Al 2 O 3 The open porosity of the composite material is 14.5% and the density is 2.09g/cm as measured by Archimedes drainage method 3 . The bending strength at room temperature was 154MPa as measured by the three-point bending test, and a typical ductile fracture mode was exhibited. After high temperature treatment at 1400 ℃ for 1h, the product resistsThe bending strength is 126MPa, and the strength retention rate is 81.8%.
Example 3
The preparation method of the fiber reinforced alumina ceramic matrix composite material comprises the following preparation processes:
(1) First, al is mixed with 2 O 3 The fiber cloth was cut to a size of 100mm×70mm×0.33mm (length×width×height), and the fiber cloth was disassembled to obtain a desired suture. Al (Al) 2 O 3 The fiber cloth is overlapped in a group of 10 pieces (the edges of the fiber cloth are aligned as much as possible), and the fiber cloth is sewn by adopting the obtained sewing thread, wherein the sewing mode is double-thread sewing, the sewing interval is 15mm multiplied by 15mm, and the fiber prefabricated member with the thickness of 3.5mm is obtained.
(2) The fiber prefabricated member is put into a muffle furnace for pretreatment, the impregnating compound on the surface of the fiber is removed, and the pretreatment conditions are as follows: inert atmosphere at 600 ℃ for 2 hours, and then cooling to room temperature along with the furnace to finish pretreatment.
(3) And placing the pretreated fiber prefabricated member into a vacuum impregnation tank, and vacuumizing until the pressure is reduced to-0.1 MPa. Introducing silica sol into an impregnation tank, and impregnating the fiber preform for 2 hours; and (3) putting the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 180 ℃, and continuously baking for 6 hours.
(4) Will complete SiO 2 The sol impregnated-solidified fiber preform is placed in a vacuum impregnation tank and vacuumized until the pressure is reduced to-0.1 MPa. Al is added with 2 O 3 The precursor solution is led into an impregnating tank to impregnate the fiber prefabricated member, and the impregnating time is 2 hours; placing the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 180 ℃, and continuously baking for 6 hours; will finish Al 2 O 3 Placing the sol impregnated-solidified fiber preform into a muffle furnace for high-temperature pyrolysis, wherein the pyrolysis temperature is 800 ℃, the pyrolysis time is 1h, and the pyrolysis atmosphere is air atmosphere, so as to initially obtain the fiber reinforced alumina ceramic matrix composite material with lower density; repeating the dipping, curing and cracking for 9 times to obtain compact Al 2 O 3f /Al 2 O 3 A composite material.
Al prepared in this example 2 O 3f /Al 2 O 3 The open porosity of the composite material is 12.5% and the density is 2.13g/cm by Archimedes drainage method 3 . The bending strength at room temperature was 148MPa as measured by the three-point bending test, and a typical ductile fracture mode was exhibited as shown in the left graph of fig. 4. After high temperature heat treatment at 1400 ℃ for 1h, the bending strength is 128MPa, and the strength retention rate is 86.5%.
As shown in FIG. 2, al of examples 1 to 3 is provided 2 O 3f /Al 2 O 3 And (5) preparing a composite material.
Comparative example 1 (1 round of dipping-curing-cracking)
Comparative example 1 differs from example 3 in that: in step (3) 1 round of dip-cure-cleave was performed, the rest of the procedure being as in example 3.
The preparation method of the fiber reinforced alumina ceramic matrix composite material comprises the following preparation processes:
(1) First, al is mixed with 2 O 3 The fiber cloth was cut to a size of 100mm×70mm×0.33mm (length×width×height), and the fiber cloth was disassembled to obtain a desired suture. Al (Al) 2 O 3 The fiber cloth is overlapped in a group of 10 pieces (the edges of the fiber cloth are aligned as much as possible), and the fiber cloth is sewn by adopting the obtained sewing thread, wherein the sewing mode is double-thread sewing, the sewing interval is 15mm multiplied by 15mm, and the fiber prefabricated member with the thickness of 3.5mm is obtained.
(2) The fiber prefabricated member is put into a muffle furnace for pretreatment, the impregnating compound on the surface of the fiber is removed, and the pretreatment conditions are as follows: inert atmosphere at 600 ℃ for 2 hours, and then cooling to room temperature along with the furnace to finish pretreatment.
(3) And placing the pretreated fiber prefabricated member into a vacuum impregnation tank, and vacuumizing until the pressure is reduced to-0.1 MPa. Introducing silica sol into an impregnation tank, and impregnating the fiber preform for 2 hours; and (3) putting the impregnated fiber prefabricated member into a baking oven for baking at 180 ℃ for 6 hours, putting the fiber prefabricated member into a muffle furnace for high-temperature pyrolysis at 700 ℃ for 1 hour, wherein the pyrolysis atmosphere is air atmosphere.
(4) Will complete SiO 2 The sol impregnated-solidified fiber preform is placed in a vacuum impregnation tank and vacuumized until the pressure is reduced to-0.1 MPa. Al is added with 2 O 3 The precursor solution is led into an impregnating tank to impregnate the fiber prefabricated member, and the impregnating time is 2 hours; placing the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 180 ℃, and continuously baking for 6 hours; will finish Al 2 O 3 Placing the sol impregnated-solidified fiber preform into a muffle furnace for high-temperature pyrolysis, wherein the pyrolysis temperature is 800 ℃, the pyrolysis time is 1h, and the pyrolysis atmosphere is air atmosphere, so as to initially obtain the fiber reinforced alumina ceramic matrix composite material with lower density; repeating the dipping, curing and cracking for 9 times to obtain compact Al 2 O 3f /Al 2 O 3 A composite material.
Al prepared in this example 2 O 3f /Al 2 O 3 The open porosity of the composite material is 12.0% and the density is 2.15g/cm by Archimedes drainage method 3 . After the SEM photograph of fig. 5 clearly goes through 1 round of dipping-curing-cracking process, the surface of the matrix is cracked more (left in fig. 5), so that the mechanical property of the material is reduced, and meanwhile, the section shows the interface between the fiber and the matrix (right in fig. 5), which indicates that the 1 round of dipping-curing-cracking is carried out, the fiber and the matrix are combined with stronger interface, no obvious gap exists, and the interface reaction between the fiber and the matrix cannot be avoided. The bending strength at room temperature was 143MPa as measured by the three-point bending test, and a typical ductile fracture mode was exhibited. After high temperature heat treatment at 1400 ℃ for 1h, the bending strength is 122MPa, and the strength retention rate is 85.3%.
By comparison, the density of the material is increased after 1 round of dipping, curing and cracking, but the damage to the fiber is increased by high-temperature treatment, the bending strength of the material and the bending strength after the high-temperature treatment are reduced to a certain extent, and meanwhile, the high-temperature cracking process is increased, so that the compounding period of the material is prolonged (1-2 days) and the cost is increased.
Comparative example 2 (Multi-round dip-cure without pyrolysis)
Comparative example 2 differs from example 3 in that: 9 rounds of dip-cure were performed in step (3), the remainder of the procedure being as in example 3.
The preparation method of the fiber reinforced alumina ceramic matrix composite material comprises the following preparation processes:
(1) First, al is mixed with 2 O 3 The fiber cloth was cut to a size of 100mm×70mm×0.33mm (length×width×height), and the fiber cloth was disassembled to obtain a desired suture. Al (Al) 2 O 3 The fiber cloth is overlapped in a group of 10 pieces (the edges of the fiber cloth are aligned as much as possible), and the fiber cloth is sewn by adopting the obtained sewing thread, wherein the sewing mode is double-thread sewing, the sewing interval is 15mm multiplied by 15mm, and the fiber prefabricated member with the thickness of 3.5mm is obtained.
(2) The fiber prefabricated member is put into a muffle furnace for pretreatment, the impregnating compound on the surface of the fiber is removed, and the pretreatment conditions are as follows: inert atmosphere at 600 ℃ for 2 hours, and then cooling to room temperature along with the furnace to finish pretreatment.
(3) And placing the pretreated fiber prefabricated member into a vacuum impregnation tank, and vacuumizing until the pressure is reduced to-0.1 MPa. Introducing silica sol into an impregnation tank, and impregnating the fiber preform for 2 hours; and (3) putting the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 180 ℃, and continuously baking for 6 hours.
(4) Will complete SiO 2 The sol impregnated-solidified fiber preform is placed in a vacuum impregnation tank and vacuumized until the pressure is reduced to-0.1 MPa. Al is added with 2 O 3 The precursor solution is led into an impregnating tank to impregnate the fiber prefabricated member, and the impregnating time is 2 hours; placing the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 180 ℃, and continuously baking for 6 hours; dip-cure was repeated 9 times.
Al prepared in this example 2 O 3f /Al 2 O 3 The composite material is not dense because the high temperature cracking process is not performed. After the impregnation-curing process is carried out again and the impregnation process is carried out again, the fiber prefabricated member is obviously softened, can not be effectively molded, the impregnation-curing is repeated for 9 times, the effect is not obviously changed, and the composite process can not prepare Al 2 O 3f /Al 2 O 3 A composite material.
Comparative example 3
Comparative example 3 is different from example 3 in that: the 1-round dip-cure-cleave process performed in step (3) uses a precursor of alumina, the remainder of the procedure being as in example 3.
The preparation method of the fiber reinforced alumina ceramic matrix composite material comprises the following preparation processes:
(1) First, al is mixed with 2 O 3 The fiber cloth was cut to a size of 100mm×70mm×0.33mm (length×width×height), and the fiber cloth was disassembled to obtain a desired suture. Al (Al) 2 O 3 The fiber cloth is overlapped in a group of 10 pieces (the edges of the fiber cloth are aligned as much as possible), and the fiber cloth is sewn by adopting the obtained sewing thread, wherein the sewing mode is double-thread sewing, the sewing interval is 15mm multiplied by 15mm, and the fiber prefabricated member with the thickness of 3.5mm is obtained.
(2) The fiber prefabricated member is put into a muffle furnace for pretreatment, the impregnating compound on the surface of the fiber is removed, and the pretreatment conditions are as follows: inert atmosphere at 600 ℃ for 2 hours, and then cooling to room temperature along with the furnace to finish pretreatment.
(3) And placing the pretreated fiber prefabricated member into a vacuum impregnation tank, and vacuumizing until the pressure is reduced to-0.1 MPa. Al is added with 2 O 3 The precursor solution is led into an impregnating tank to impregnate the fiber prefabricated member, and the impregnating time is 2 hours; placing the impregnated fiber prefabricated member into a baking oven for baking, wherein the baking temperature is 180 ℃, and continuously baking for 6 hours; will finish Al 2 O 3 Placing the sol impregnated-solidified fiber preform into a muffle furnace for high-temperature pyrolysis, wherein the pyrolysis temperature is 800 ℃, the pyrolysis time is 1h, and the pyrolysis atmosphere is air atmosphere, so as to initially obtain the fiber reinforced alumina ceramic matrix composite material with lower density; repeating the dipping, curing and cracking for 9 times to obtain compact Al 2 O 3f /Al 2 O 3 A composite material.
Al prepared in this example 2 O 3f /Al 2 O 3 The open porosity of the composite material is 13.0% and the density is 2.18g/cm as measured by Archimedes drainage method 3 . The bending strength at room temperature was 133MPa as measured by the three-point bending test, and a typical brittle fracture mode was exhibited. High temperature heat treatment at 1400 ℃ for 1hAfter the treatment, the flexural strength was 102MPa and the strength retention was 76.7%.
By comparison, it was found that the density of the material increased after no interfacial coating treatment, but Al 2 O 3f /Al 2 O 3 The composite material exhibited a typical brittle fracture mode, as shown in the right hand graph of fig. 4, which was analyzed primarily because the fiber to matrix interface bond strength was too high.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (10)
1. A method for preparing a fiber reinforced alumina ceramic matrix composite, the method comprising the steps of:
s1, performing high-temperature heat treatment on a fiber prefabricated member to obtain a fiber prefabricated member to be impregnated;
s2, dipping, drying and solidifying the fiber prefabricated member to be dipped by adopting silica sol to obtain a fiber prefabricated member with a silica interface layer;
s3, adopting an alumina precursor solution to impregnate, dry and solidify and crack a fiber preform with a silica interface layer at high temperature to obtain a fiber reinforced alumina ceramic matrix composite semi-finished product;
s4, carrying out dipping, drying, curing and high-temperature cracking on the semi-finished product of the fiber reinforced alumina ceramic matrix composite for 5-10 times until the weight gain rate of the weight of the fiber reinforced alumina ceramic matrix composite is lower than a preset value compared with the weight gain rate of the fiber reinforced alumina ceramic matrix composite after the previous high-temperature cracking, thus obtaining the finished product of the fiber reinforced alumina ceramic matrix composite.
2. The method for producing a fiber-reinforced alumina ceramic matrix composite according to claim 1, wherein in step S1, the conditions of the high-temperature heat treatment are: the temperature is 500-800 ℃, the inert atmosphere is used, and the heat preservation time is 0.5-2 h.
3. The method for preparing a fiber reinforced alumina ceramic matrix composite according to claim 1, wherein in the step S2, the operation of sequentially impregnating and drying the fiber preform to be impregnated is performed 1 time.
4. The method for preparing a fiber reinforced alumina ceramic matrix composite according to claim 1, wherein in the steps S2 to S4, the impregnation mode is vacuum impregnation, the pressure is reduced to-0.1 MPa, and the impregnation time is 2 to 8 hours.
5. The method for preparing a fiber reinforced alumina ceramic matrix composite according to claim 1, wherein in the steps S2 to S4, the curing temperature is 150 ℃ to 200 ℃ and the heat preservation time is 2h to 8h.
6. The method for preparing the fiber reinforced alumina ceramic matrix composite according to claim 1, wherein in the steps S3 to S4, the high-temperature cracking temperature is 700 ℃ to 900 ℃, the heat preservation time is 0.5h to 2h, and the cracking atmosphere is air or inert atmosphere.
7. The method for producing a fiber-reinforced alumina ceramic matrix composite according to claim 1, wherein the preset value in step S4 is 1wt%.
8. The method for preparing a fiber reinforced alumina ceramic matrix composite according to claim 1, wherein in the step S4, the number of times is 5 to 10 times.
9. The method for preparing a fiber reinforced alumina ceramic matrix composite according to claim 1, further comprising, prior to step S1:
cutting the alumina fiber cloth according to the required size;
disassembling the alumina fiber cloth to obtain a required suture line;
and sewing the cut alumina fiber cloth by adopting a suture line to obtain a fiber prefabricated member.
10. The method of producing a fiber reinforced alumina ceramic matrix composite according to claim 9, wherein the stitching is double stitching with a stitching pitch of 3mm x 3mm to 15mm x 15mm.
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