CN110183216A - High-temperature-resistant Al2O3Base composite material and densification preparation method thereof - Google Patents
High-temperature-resistant Al2O3Base composite material and densification preparation method thereof Download PDFInfo
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- CN110183216A CN110183216A CN201910466505.XA CN201910466505A CN110183216A CN 110183216 A CN110183216 A CN 110183216A CN 201910466505 A CN201910466505 A CN 201910466505A CN 110183216 A CN110183216 A CN 110183216A
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- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
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Abstract
The invention discloses high-temperature resistant Al2O3The method uses multilayer inorganic fiber cloth or fabric as reinforcement, firstly carries out pretreatment on the inorganic fiber cloth or fabric raw material to obtain the reinforcement meeting the requirement, then fills alumina sol into the reinforcement, carries out gelation treatment and high temperature cracking, then repeats the steps of dipping-gelling-cracking until the weight gain ratio of the alumina weaving piece is less than 1%, and obtains the high temperature resistant Al2O3A base composite material. Compared with the prior art, the preparation method provided by the invention has the advantages of simple preparation process, low cost and obvious effect of reducing the porosity of the product; the invention provides high-temperature resistant Al2O3The base composite material takes inorganic fiber cloth or fabric as a reinforcement and alumina sol as a matrix; of said reinforcement and said matrixThe mass ratio is (10:1) - (1:1), the composite material has excellent temperature resistance, and can be used for a long time in a high-temperature oxidation environment; high strength, high bearing capacity and low porosity.
Description
Technical field
The present invention relates to sol-gel methods to prepare Al2O3Based composites technical field, especially a kind of high temperature resistant Al2O3
Based composites and its densification preparation method.
Background technique
Continuous fiber toughening ceramic based composites (CFRCMCs) are due to its excellent performance, such as high-intensitive, Gao Mo
Amount, high tenacity, corrosion-resistant etc., by the favor of domestic and international scientific research personnel, in terms of aerospace, advanced weaponry, ship, nuclear energy
All it is widely used.The continuous fiber toughening ceramic based composites of early stage are mainly carried out in C, SiC ceramic based composites,
The fiber of use is also C, SiC fiber, and typical composite material is exactly C/C composite material, C/SiC composite material and SiC/SiC.
But this kind of non-oxide ceramics based composites have a fatal defect, are exactly that can not grow in the environment of high-temperature oxydation
Time uses, because its matrix is particularly easy to occur oxidation to fail, this makes non-oxide ceramics based composites in height
Application under warm oxidation environment is limited by very large.
As the important branch of ceramic matric composite, (oxide/oxide is compound for Oxide/Oxide composite material
Material) paid attention to due to the development of oxide fibre.Oxide ceramics has excellent high temperature resistant and corrosion resistance, can
To be used for a long time under high-temperature oxidation environment.Non-oxide ceramics matrix is replaced using oxide ceramics matrix, it can be one
Determine the inoxidizability performance that degree improves composite material, ceramic matric composite can be made to apply in aerospace field heat structure
Material becomes possibility.
Al2O3With the excellent properties such as high intensity, high-modulus, corrosion-resistant, high temperature resistant, anti-oxidant, have huge development latent
Power.Simultaneously as Al2O3With excellent high temperature resistant and corrosion resistance, can be used for a long time under high-temperature oxidation environment,
With Al2O3For the oxide/oxide ceramic matric composite of matrix preparation antioxygenic property and dielectric properties are excellent, structure
Stability is high, the high-temperature service service life is long, is ideal structure and functional material applied to high temperature aerobic environment.
Prepare Al2O3Based composites are critical that Al2O3Basis material is uniformly substantially filled in fiber braid,
There are certain intervals between fibre bundle, tend to form closed pore during the preparation process, lead to the whole porosity of composite material
It is higher, and then the performance (mechanical property and dielectric properties) of material is influenced, therefore, it is necessary to take suitable technique to prepare Al2O3
Based composites.Tradition preparation Al2O3The method of based composites is usually slurry infiltration-winding/heat pressing process (SI-W/HP),
The Al prepared using this method2O3Based composites hole is more, commonly referred to as porous Al2O3Based composites.
Summary of the invention
The present invention provides a kind of high temperature resistant Al2O3Based composites and its densification preparation method, for overcoming the prior art
Middle Al2O3The defects of product porosity that based composites preparation method is prepared is high, realizes the Al being prepared2O3Base is multiple
Condensation material intensity with higher and good densification effect, porosity are low.
To achieve the above object, the present invention proposes a kind of high temperature resistant Al2O3Based composites densify preparation method, including
Following steps:
(1) inorfil cloth or fabric cut, degumming, be stacked to several layers, sutured；
(2) under vacuum conditions, the inorfil cloth or fabric after suture is impregnated, maceration extract is that aluminium oxide is molten
Glue obtains aluminium oxide braided part；
(3) aluminium oxide braided part is subjected to gelation processing, then cooled and solidified at room temperature；
(4) Pintsch process will be carried out by the aluminium oxide braided part of step (3)；
(5) step (2)~(4) are repeated until the rate of body weight gain of aluminium oxide braided part obtains high temperature resistant Al less than 1%2O3Base is multiple
Condensation material.
To achieve the above object, the present invention also proposes a kind of high temperature resistant Al2O3Based composites, the Al2O3Base composite wood
Material is matrix by reinforcement, alumina sol of inorfil cloth or fabric；The mass ratio of the reinforcement and described matrix is
(10:1)~(1:1)；The Al2O3The porosity of based composites is less than 20%.
Compared with prior art, the beneficial effects of the present invention are as follows:
1, high temperature resistant Al provided by the invention2O3Based composites densify preparation method, with multilayer inorfil cloth or knit
Object is reinforcement, first is pre-processed to obtain satisfactory reinforcement to inorfil cloth or fabric raw material, then to enhancing
Filling alumina sol in vivo is passing through gelation processing, Pintsch process, it is straight to repeat dipping-gel-cleavage step later
To aluminium oxide braided part rate of body weight gain less than 1%, obtain high temperature resistant Al2O3Based composites.The inorfil cloth that this method uses
Or textile source is wide, cheap, reduces preparation cost；Preparation process is simple, and to reducing, product porosity effect is bright
It is aobvious.
2, high temperature resistant Al provided by the invention2O3Based composites, the Al2O3Based composites with inorfil cloth or
Fabric is reinforcement, alumina sol is matrix；The mass ratio of the reinforcement and described matrix is (10:1)~(1:1)；Institute
State Al2O3The porosity of based composites is less than 20%.The composite material heat resistance is excellent, can be in the environment of high-temperature oxydation
It uses for a long time；Intensity is high, bearing capacity is strong, porosity is low.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
The structure shown according to these attached drawings obtains other attached drawings.
Fig. 1 is high temperature resistant Al provided by the invention2O3Based composites densify preparation method flow diagram.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
It in addition, the technical solution between each embodiment of the present invention can be combined with each other, but must be general with this field
Based on logical technical staff can be realized, it will be understood that when the combination of technical solution appearance is conflicting or cannot achieve this
The combination of technical solution is not present, also not the present invention claims protection scope within.
Without specified otherwise, used drug/reagent is commercially available.
The present invention proposes a kind of high temperature resistant Al2O3Based composites densify preparation method, as shown in Figure 1, including following step
It is rapid:
(1) inorfil cloth or fabric cut, degumming, be stacked to several layers, sutured, obtain fiber preform；
Preferably, in the step (1), the thickness in monolayer of the inorfil cloth or fabric is 0.1~2.0mm；Fiber
The thickness of prefabricated component is determined by adjusting the number of plies of fiber cloth or fabric, to control the thickness of composite material face.
The inorfil cloth or fabric is one of silicon oxide fibre, alumina fibre or mullite fiber.
Preferably, the temperature of the degumming is 500~600 DEG C, and the time is 1~3h, and the purpose of degumming process is that removal is fine
The organic gel in dimension table face is conducive to solution dipping；Using the method for needle-penetration thorn, the spacing of suture is 5~10mm for the suture.
Needle-penetration prickseam closes design, in addition puncture line, suture are flexible, ensure that the flexibility of material, in a compressed state, is not in
The problems such as fractureing or ejecting；It is very smooth without apparent protrusion or dent, panel surface that needle-penetration pierces line.Spacing should control
Suitably, the overstocked fiber cloth or fabric that will lead to can not be sutured effectively, and the mechanical property of excessively dilute composite material that will lead to preparation becomes
Difference.
(2) under vacuum conditions, the inorfil cloth or fabric after suture is impregnated, maceration extract is that aluminium oxide is molten
Glue obtains aluminium oxide braided part；In impregnating autoclave pressure be lower than -0.1MPa when keep at least 10min, when in tank vacuum pressure value without
Alumina sol is introduced when significant change.
Preferably, in the step (2), the dipping guarantees that dipping is abundant to impregnate 3~6h at room temperature.
(3) aluminium oxide braided part is subjected to gelation processing, alumina sol is converted into gel, then cools down at room temperature
Solidification generates alumina substrate；
Preferably, in the step (3), gelation processing for the rate of 5~10 DEG C/min by temperature from room temperature
100~300 DEG C are warming up to, and keeps the temperature 1~3h at 100~300 DEG C.Under the described conditions, gelation treatment effect is best.
(4) Pintsch process will be carried out by the aluminium oxide braided part of step (3)；
Preferably, in the step (4), the Pintsch process is by temperature with the rate of 5~10 DEG C/min from room temperature liter
Temperature keeps the temperature 0.5~1h to 900~1100 DEG C at 900~1100 DEG C.Composite material is prepared at 900~1100 DEG C to fibre
It is smaller to tie up original performance influence；Under the described conditions, lytic effect is best.
(5) step (2)~(4) are repeated until the rate of body weight gain of aluminium oxide braided part obtains high temperature resistant Al less than 1%2O3Base is multiple
Condensation material.It repeats the operation several times, so that the porosity of resulting materials significantly reduces.
Preferably, in the step (5), the duplicate number is 10~15 times.
High temperature resistant Al provided by the invention2O3Based composites densify preparation method, with multilayer inorfil cloth or fabric
For matrix, first inorfil cloth or fabric raw material is pre-processed to obtain satisfactory matrix, then be filled into matrix
Alumina sol is passing through gelation processing, Pintsch process, repeats dipping-gel-cleavage step later until aluminium oxide
The rate of body weight gain of braided part obtains high temperature resistant Al less than 1%2O3Based composites.The inorfil cloth or fabric that this method uses is former
Expect that source is wide, cheap, reduces preparation cost；Preparation process is simple, and to reducing, product porosity effect is obvious.
The present invention also proposes a kind of high temperature resistant Al2O3Based composites, the Al2O3Based composites are with inorfil cloth
Or fabric is reinforcement, alumina sol is matrix；The mass ratio of the reinforcement and described matrix is (10:1)~(1:1)；
The Al2O3The porosity of based composites is 17.5~19.5% less than 20%.
Preferably, 1.80~1.99g/cm of density of the composite material3, fracture elongation 1.3~1.5%, toughness 7~
10MPa·m1/2, 1500 DEG C of bending strength 70~90MPa, 1500 DEG C of 28~48GPa of bending modulus, suture direction bending strength
127~147MPa, suture direction 30~50GPa of bending modulus, thickness direction 120~150MPa of compressive strength, thickness direction pressure
Contracting 9~10GPa of modulus can tolerate 1400 DEG C under the long-time of 20~30min.
Embodiment one
The present embodiment provides high temperature resistant Al2O3Based composites, using alumina fibre cloth as matrix, plate thickness 3mm.
Preparation method the following steps are included:
(1) alumina fibre cloth is cut to the square of 250 × 250mm, by the alumina fibre cloth after cutting 500
Then 9 layers of alumina fibre cloth are piled up by degumming process 3h at DEG C, the aluminium oxide folded with alumina fibre line counterweight is fine
Wei Bu is sutured, and suture spacing is 5mm, then fixes the alumina fibre prefabricated component sutured with high-temperature alloy mold
It clamps；
(2) fiber preform sutured is put into vacuum impregnation tank, it is vacuumized, to vacuum impregnation pressure inside the tank
0.5h is kept when lower than -0.1MPa, introduces alumina sol, carries out mass-impregnation, dip time 6h；
(3) it by the resulting sufficient aluminium oxide braided part of dipping of step (2), is put into baking oven and dries, the colloidal sol of dipping fills
Segregate glue, baking oven with the rate of 10 DEG C/min by temperature from room temperature to 150 DEG C, and keep the temperature 3h at 150 DEG C；
(4) will through step (3), treated that alumina fibre braided part is put into horse kettle furnace cracks, with 10 DEG C/min
Rate by temperature from room temperature to 1100 DEG C, keep the temperature 1h at 1100 DEG C；
(5) repeat the above steps total 12 times of (2)~(4), until the rate of body weight gain of composite material is less than 1%, obtains resistance to height
Warm Al2O3Based composites.
Prepared composite thin plate is machined, size needed for obtaining various tests.Prepared is resistance to
High temperature Al2O3Based composites have good intensity and toughness, and thin sheet surface flatness reaches 0.1mm, and suture is without obvious
Protrusion or dent.The present embodiment high temperature resistant Al2O3The basic performance of based composites is shown in Table 1.
Embodiment two
The present embodiment provides high temperature resistant Al2O3Based composites, using silicon oxide fibre cloth as matrix, plate thickness 3mm.
Preparation method the following steps are included:
(1) silicon oxide fibre cloth is cut to the square of 220 × 220mm, by the silicon oxide fibre cloth after cutting 550
Then 10 layers of silicon oxide fibre cloth are piled up by degumming process 2h at DEG C, the silica folded with silicon oxide fibre line counterweight
Fiber cloth is sutured, and suture spacing is 8mm, then consolidates the silicon oxide fibre prefabricated component high-temperature alloy mold sutured
Clamp is tight；
(2) fiber preform sutured is put into vacuum impregnation tank, it is vacuumized, to vacuum impregnation pressure inside the tank
0.5h is kept when lower than -0.1MPa, introduces alumina sol, carries out mass-impregnation, dip time 3h；
(3) it by the resulting sufficient silica braided part of dipping of step (2), is put into baking oven and dries, the colloidal sol of dipping fills
Segregate glue, baking oven with the rate of 5 DEG C/min by temperature from room temperature to 300 DEG C, and keep the temperature 1h at 300 DEG C；
(4) will through step (3), treated that silicon oxide fibre braided part is put into horse kettle furnace cracks, with 5 DEG C/min
Rate by temperature from room temperature to 900 DEG C, keep the temperature 1h at 900 DEG C；
(5) repeat the above steps total 15 times of (2)~(4), until the rate of body weight gain of composite material is less than 1%, obtains resistance to height
Warm Al2O3Based composites.
Prepared composite thin plate is machined, size needed for obtaining various tests.Prepared is resistance to
High temperature Al2O3Based composites have good intensity and toughness, and thin sheet surface flatness reaches 0.1mm, and suture is without obvious
Protrusion or dent.The present embodiment high temperature resistant Al2O3The basic performance of based composites is shown in Table 2.
Embodiment three
The present embodiment provides high temperature resistant Al2O3Based composites, using mullite fiber cloth as matrix, plate thickness 2mm.
Preparation method the following steps are included:
(1) mullite fiber cloth is cut to the square of 330 × 330mm, by the mullite fiber cloth after cutting 600
Then 10 layers of mullite fiber cloth are piled up by degumming process 1h at DEG C, the mullite folded with mullite fiber line counterweight
Fiber cloth is sutured, and suture spacing is 10mm, the mullite fiber prefabricated component high-temperature alloy mold that will then suture
It fixes to clamp；
(2) fiber preform sutured is put into vacuum impregnation tank, it is vacuumized, to vacuum impregnation pressure inside the tank
0.5h is kept when lower than -0.1MPa, introduces alumina sol, carries out mass-impregnation, dip time 4h；
(3) it by the resulting sufficient mullite braided part of dipping of step (2), is put into baking oven and dries, the colloidal sol of dipping fills
Segregate glue, baking oven with the rate of 8 DEG C/min by temperature from room temperature to 100 DEG C, and keep the temperature 3h at 100 DEG C；
(4) will through step (3), treated that mullite fiber braided part is put into horse kettle furnace cracks, with 8 DEG C/min
Rate by temperature from room temperature to 1000 DEG C, keep the temperature 0.5h at 1000 DEG C；
(5) repeat the above steps total 15 times of (2)~(4), until the rate of body weight gain of composite material is less than 1%, obtains resistance to height
Warm Al2O3Based composites.
Prepared composite thin plate is machined, size needed for obtaining various tests.Prepared is resistance to
High temperature Al2O3Based composites have good intensity and toughness, and thin sheet surface flatness reaches 0.1mm, and suture is without obvious
Protrusion or dent.The present embodiment high temperature resistant Al2O3The basic performance of based composites is shown in Table 3.
Comparative example one
This comparative example provides a kind of tradition preparation Al2O3The method of based composites, usually slurry infiltration-heat pressing process
(SI-W/HP), with SiO2Fiber cloth is matrix, and product design is with a thickness of 3mm.Preparation method the following steps are included:
(1) slurry infiltrates: by 9 layers of SiO2Fiber is arranged in vacuum tank, vacuum suck Al2O3Colloidal sol impregnates 2h,
(2) heat pressing process: by SiO obtained by step (1)2Fiber cloth heat resisting steel mold cramping, setting, will with a thickness of 3mm
Prefabricated component is placed in hot pressing furnace and is heat-treated, and is heated to 1000 DEG C with the rate of 10 DEG C/min, and pressure is maintained at 1MPa,
Soaking time is 2h；It is taken out after natural cooling；
(3) the slurry infiltration-heat pressing process 6 times repeatedly；Obtain Al2O3Based composites.The Al that this comparative example provides2O3
The basic performance of based composites is shown in Table 4.
The Al of 1 embodiment one of table preparation2O3Based composites basic performance
The Al of 2 embodiment two of table preparation2O3Based composites basic performance
The Al of 3 embodiment three of table preparation2O3Based composites basic performance
4 comparative example one of table is prepared into Al2O3Based composites basic performance
It can be seen that high temperature resistant Al provided by the invention from above-described embodiment and comparative example2O3Based composites densification system
Preparation Method simple process is obvious (being lower than 20%) to product porosity effect is reduced compared with prior art；It is provided by the invention
High temperature resistant Al2O3Based composites can use for a long time in the environment of high-temperature oxydation, and porosity is low, mechanical property and dielectricity
It can be excellent.
Preparation method provided by the invention is expected to become large-scale production preparation Al in industrial circle2O3Based composites
Effective ways, products application obtained have a extensive future.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
It is included in other related technical areas in scope of patent protection of the invention.
Claims (10)
1. a kind of high temperature resistant Al2O3Based composites densify preparation method, which comprises the following steps:
(1) inorfil cloth or fabric cut, degumming, be stacked to several layers, sutured；
(2) under vacuum conditions, the inorfil cloth or fabric after suture is impregnated, maceration extract is alumina sol, is obtained
To aluminium oxide braided part；
(3) aluminium oxide braided part is subjected to gelation processing, then cooled and solidified at room temperature；
(4) Pintsch process will be carried out by the aluminium oxide braided part of step (3)；
(5) step (2)~(4) are repeated until the rate of body weight gain of aluminium oxide braided part obtains high temperature resistant Al less than 1%2O3Base composite wood
Material.
2. a kind of high temperature resistant Al as described in claim 12O3Based composites densify preparation method, which is characterized in that described
In step (1), the thickness in monolayer of the inorfil cloth or fabric is 0.1~2.0mm.
3. a kind of high temperature resistant Al as claimed in claim 22O3Based composites densify preparation method, which is characterized in that described
Inorfil cloth or fabric is one of silicon oxide fibre, alumina fibre or mullite fiber.
4. a kind of high temperature resistant Al as described in claim 12O3Based composites densify preparation method, which is characterized in that described
In step (1), the temperature of the degumming is 500~600 DEG C, and the time is 1~3h；The side that the suture is pierced or punctured using needle
Method, the spacing of suture are 5~10mm.
5. a kind of high temperature resistant Al as described in claim 12O3Based composites densify preparation method, which is characterized in that described
In step (2), the dipping is 3~6h of dipping at room temperature.
6. a kind of high temperature resistant Al as described in claim 12O3Based composites densify preparation method, which is characterized in that described
In step (3), the gelation processing is by temperature with the rate of 5~10 DEG C/min from room temperature to 100~300 DEG C, and
1~3h is kept the temperature at 100~300 DEG C.
7. a kind of high temperature resistant Al as described in claim 12O3Based composites densify preparation method, which is characterized in that described
In step (4), the Pintsch process is by temperature with the rate of 5~10 DEG C/min from room temperature to 900~1100 DEG C, and
0.5~1h is kept the temperature at 900~1100 DEG C.
8. a kind of high temperature resistant Al as described in claim 12O3Based composites densify preparation method, which is characterized in that described
In step (5), the duplicate number is 10~15 times.
9. a kind of high temperature resistant Al2O3Based composites, which is characterized in that the Al2O3Based composites are with inorfil cloth or knit
Object is reinforcement, alumina sol is matrix；The mass ratio of the reinforcement and described matrix is (10:1)~(1:1)；It is described
Al2O3The porosity of based composites is less than 20%.
10. a kind of high temperature resistant Al as claimed in claim 92O3Based composites, which is characterized in that the composite material it is close
Spend 1.80~1.99g/cm3, fracture elongation 1.3~1.5%, 7~10MPam of toughness1/2, 1500 DEG C of bending strengths 70~
90MPa, 1500 DEG C of 28~48GPa of bending modulus, suture direction 127~147MPa of bending strength, suture direction bending modulus 30
~50GPa, thickness direction 120~150MPa of compressive strength, thickness direction 9~10GPa of compression modulus, in the length of 20~30min
It can tolerate 1400 DEG C under time.
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