CN109664568A - A kind of wideband wave transparent multilayered structure ceramic matric composite and preparation method thereof - Google Patents
A kind of wideband wave transparent multilayered structure ceramic matric composite and preparation method thereof Download PDFInfo
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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Abstract
The present invention relates to a kind of wideband wave transparent multilayered structure ceramic matric composites and preparation method thereof, belong to technical field of composite materials.The multilayered structure ceramic matric composite is laminated by the inorganic wave transparent fiber reinforced ceramic matrix composites of odd-level, and the dielectric constant of the inorganic wave transparent fiber reinforced ceramic matrix composites of odd-level is successively increased by outer layer to middle layer, is adhesively fixed between each layer by inorganic wave penetrating paint.The wideband wave transparent multilayered structure ceramic matric composite, up to 80% or more, and can use for a long time in X/Ku/Ka wave band (bandwidth highest is close to 50G) transmitance under 1000 DEG C or more hot environments, highly reliable.
Description
Technical field
The present invention relates to a kind of wideband wave transparent multilayered structure ceramic matric composites and preparation method thereof, belong to composite material
Technical field.
Background technique
Wide-frequency wave-transparent composite material mainly uses multilayer organic media (covering, low density foam or honeycomb sandwich layer etc.) at present
Combined sandwich is limited by organic material high temperature resistance, is not used to 600 DEG C or more of applied at elevated temperature environment, is needed
Upgrade to the better inorganic of high temperature resistance.
Currently, the multiple layer combination mode of the research over-borrowing mirror organic interlayer structure of inorganic wideband electromagnetic wave transparent material, is developed with stone
Low-density inorganic dielectric material based on English, silicon nitride, aluminium oxide, mullite etc. as low dielectric sandwich layer, with it is high-intensitive compared with
Densified thin layer substitutes organic media, as covering to improve the use temperature of wideband electromagnetic wave transparent material, but the width of this three-decker
Frequency wave transparent limited capacity (bandwidth is only 1~2G or so) is difficult to meet high-temperature wide-frequency wave transparent needs.And it is general between layers
It is connected using organic binder, solidification temperature is low, and (300 DEG C or more) organic matter can decompose, be carbonized under high temperature, high temperature reliability
Difference.
Summary of the invention
The purpose of the present invention is to provide a kind of wideband wave transparent multilayered structure ceramic matric composite and preparation method thereof, institutes
It is reachable in X/Ku/Ka wave band (bandwidth highest is close to 50G) transmitance to state wideband wave transparent multilayered structure ceramic matric composite
80% or more, and can be used for a long time under 1000 DEG C or more hot environments, it is highly reliable.
For achieving the above object, the invention provides the following technical scheme:
A kind of wideband wave transparent multilayered structure ceramic matric composite, it is compound by the inorganic wave transparent fiber reinforced ceramic-base of odd-level
Material is laminated, and the dielectric constant of the inorganic wave transparent fiber reinforced ceramic matrix composites of the odd-level is by outer layer to centre
Layer successively increases, and is adhesively fixed between each layer by inorganic wave penetrating paint.
In an alternative embodiment, it is laminated by 5 layers of inorganic wave transparent fiber reinforced ceramic matrix composites, and middle layer
Dielectric constant is 2.8~4.0, and the dielectric constant with the middle layer adjacent two layers is 1.8~2.8, outermost two layers of dielectric constant
It is 1.2~1.8.
In an alternative embodiment, the inorganic wave penetrating paint is dispersed in silica solution for inorganic wave transparent ceramic powder and is formed
Suspension.
In an alternative embodiment, the inorganic wave transparent ceramic powder be boron oxide, aluminium oxide, yttrium oxide, silicon nitride or
At least one of boron nitride powder.
In an alternative embodiment, purity >=99.9% of the silica solution, the mass content of silica is 30~60%;
Purity >=99% of the inorganic wave transparent ceramic powder, the quality of the inorganic wave transparent ceramic powder are the siliconoxide mass
5%~20%.
In an alternative embodiment, each thickness degree is 3.0~5.0mm.
A kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite, comprising the following steps:
(1) by the inorganic wave transparent fiber reinforced ceramic matrix composites of odd-level according to dielectric constant by outer layer to middle layer according to
Secondary increased sequence stacks, and inorganic wave penetrating paint is applied between adjacent two layers before stacking;
(2) applying pressure is in close contact each layer, is heat-treated, obtains multilayered structure ceramic matric composite.
In an alternative embodiment, 5 layers of inorganic wave transparent fiber reinforced ceramic matrix composites are laminated in step (1), and
Inter level dielectric constant is 2.8~4.0, and the dielectric constant with the middle layer adjacent two layers is 1.8~2.8, outermost two layers of Jie
Electric constant is 1.2~1.8.
In an alternative embodiment, step (1) the inorganic wave penetrating paint is that be dispersed in silicon molten for inorganic wave transparent ceramic powder
The suspension formed in glue.
In an alternative embodiment, the inorganic wave transparent ceramic powder be boron oxide, aluminium oxide, yttrium oxide, silicon nitride or
At least one of boron nitride powder.
In an alternative embodiment, purity >=99.9% of the silica solution, the mass content of silica is 30~60%;
Purity >=99% of the inorganic wave transparent ceramic powder, the quality of the inorganic wave transparent ceramic powder are the siliconoxide mass
5%~20%.
In an alternative embodiment, the inorganic wave penetrating paint is applied by the way of spraying, quantity for spray 100
~500g/m2。
In an alternative embodiment, each thickness degree is 3.0~5.0mm in step (1).
Applying 0.1~0.5MPa pressure in an alternative embodiment, in step (2) is in close contact each layer.
In an alternative embodiment, heat treatment described in step (2), temperature be 600~1200 DEG C, soaking time be 60~
180min。
In an alternative embodiment, 600~1200 DEG C are warming up to the heating rate of 1~5 DEG C/min in step (2);It protects
After temperature, 100 DEG C are cooled to the rate of 0.2~0.5 DEG C/min.
Compared with prior art, the present invention has the following advantages:
(1) multilayered structure ceramic matric composite provided in an embodiment of the present invention, by according to dielectric constant from outside to inside
Sequence incremented by successively stacks multi-layer ceramics based composites, and is bonded each layer by inorganic coating, the multilayered structure made
Ceramic matric composite has excellent wideband wave transparent performance, in X/Ku/Ka wave band transmitance up to 80% or more, and can be
It is used for a long time under 1000 DEG C or more hot environments;
(2) the dielectric constant proportion of five layer material provided in an embodiment of the present invention had both considered dielectric gradual change and has widened wave transparent band
Width, it is contemplated that carrying, being thermally matched and heat-insulated, wherein middle layer is principal carrier sheet, and density and intensity are higher, is connected with middle layer
Two layers connect is transition zone, and the thermal expansion coefficient difference between middle layer and outermost layer is larger, and transition zone can reduce its thermal mismatching,
Outermost layer is mainly thermal insulation layer;
(3) present invention is that the inorganic coating that embodiment provides can keep excellent dielectricity at -50 DEG C~1000 DEG C
Can, wave transparent performance is not influenced, and can play reliable connection function.
Detailed description of the invention
Fig. 1 is composite material and preparation method thereof flow chart provided in an embodiment of the present invention;
Fig. 2 is that the five-layer structure combination that inventive embodiments provide and inorganic coating are bonded schematic diagram;
Fig. 3 is wideband wave transparent performance of the five layers of component of typical case that provide of embodiment 3 in X/Ku/Ka wave band;
Fig. 4 is the component diagrammatic cross-section that embodiment 3 provides.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments:
The embodiment of the invention provides a kind of wideband wave transparent multilayered structure ceramic matric composites, by the inorganic wave transparent of odd-level
Fiber reinforced ceramic matrix composites is laminated, and Jie of the inorganic wave transparent fiber reinforced ceramic matrix composites of the odd-level
Electric constant is successively increased by outer layer to middle layer, is adhesively fixed between each layer by inorganic wave penetrating paint.
Specifically, in the embodiment of the present invention, preferably 5 layers, 7 layers and 9 layers, more preferable 5 layers of odd-level;The inorganic wave transparent is fine
Tie up preferred quartz fibre, silicon nitride fiber, mullite fiber, alumina fibre, silicon boron nitrogen fiber, boron nitride fiber or high silicon oxygen
At least one of fiber;The embodiment of the present invention can by change wave transparent fiber type and/or adjust matrix content come
Adjust the dielectric constant of each layer;In the embodiment of the present invention, using middle layer as symmetrical centre, two layers symmetrical of dielectric constant can
It can also be different with identical, it is preferably identical;Each thickness degree is preferably identical, more preferably 3.0~5.0mm.
Multilayered structure ceramic matric composite provided in an embodiment of the present invention, by according to dielectric constant from outside to inside successively
Incremental sequence stacks multi-layer ceramics based composites, and is bonded each layer by inorganic coating, the multilayered structure ceramics made
Based composites have excellent wideband wave transparent performance, in X/Ku/Ka wave band transmitance up to 80% or more, and can be at 1000 DEG C
It is used for a long time under the above hot environment.
In an alternative embodiment, it is laminated by 5 layers of inorganic wave transparent fiber reinforced ceramic matrix composites, and middle layer
Dielectric constant is 2.8~4.0, and the dielectric constant with the middle layer adjacent two layers is 1.8~2.8, outermost two layers of dielectric constant
It is 1.2~1.8.The dielectric constant proportion of five layer material provided in an embodiment of the present invention had both considered dielectric gradual change and has widened wave transparent band
Width, it is contemplated that carrying, being thermally matched and heat-insulated, wherein middle layer is principal carrier sheet, and density and intensity are higher, is connected with middle layer
Two layers connect is transition zone, and the thermal expansion coefficient difference between middle layer and outermost layer is larger, and transition zone can reduce its thermal mismatching,
Outermost layer is mainly thermal insulation layer;
In an alternative embodiment, the inorganic wave penetrating paint is dispersed in silica solution for inorganic wave transparent ceramic powder and is formed
Suspension.Wherein, the preferred boron oxide of the inorganic wave transparent ceramic powder, aluminium oxide, yttrium oxide, silicon nitride or boron nitride powder
At least one of, it can be dispersed in silica solution by modes such as ball milling, stirrings.
Specifically, the silica solution purity preferably >=99.9%, the mass content of silica preferably 30~60%;It is described
Preferably >=99%, the quality of the inorganic wave transparent ceramic powder is preferably that the oxidation is siliceous to the purity of inorganic wave transparent ceramic powder
The 5%~20% of amount.The inorganic coating can keep excellent dielectric properties at -50 DEG C~1000 DEG C, not influence wave
Can, and reliable connection function can be played.
The embodiment of the invention also provides a kind of preparation methods of wideband wave transparent multilayered structure ceramic matric composite, including
Following steps:
(1) by the inorganic wave transparent fiber reinforced ceramic matrix composites of odd-level according to dielectric constant by outer layer to middle layer according to
Secondary increased sequence stacks, and inorganic wave penetrating paint is applied between adjacent two layers before stacking;
(2) applying pressure is in close contact each layer, is heat-treated, obtains multilayered structure ceramic matric composite.
The embodiment of the present invention is used to prepare wideband wave transparent multilayered structure ceramic matric composite provided by the above embodiment, has
Referring to above-described embodiment, details are not described herein for the description of pass product.
In an alternative embodiment, 5 layers of ceramic matric composite are laminated in step (1), and inter level dielectric constant is
2.8~4.0, the dielectric constant with the middle layer adjacent two layers is 1.8~2.8, and outermost two layers of dielectric constant is 1.2~1.8.
In an alternative embodiment, the inorganic wave penetrating paint is dispersed in silica solution for inorganic wave transparent ceramic powder and is formed
Suspension.Wherein, the preferred boron oxide of the inorganic wave transparent ceramic powder, aluminium oxide, yttrium oxide, silicon nitride or boron nitride powder
At least one of.
Specifically, the silica solution purity preferably >=99.9%, the mass content of silica preferably 30~60%;It is described
The purity of inorganic wave transparent ceramic powder preferably >=99%, mass content of the inorganic wave transparent ceramic powder in the silica solution
It is preferred that 5%~20%.
In one embodiment, the inorganic wave penetrating paint is applied by the way of spraying, quantity for spray 100
~500g/m2;The range can guarantee that the coating after preparation has good adhesive strength, too low, be likely to hole occur, both
Adhesive strength is reduced, and weakens wave transparent performance, it is excessively high, make thickness of adhibited layer higher, is easy embrittlement;
Applying 0.1~0.5MPa pressure in an alternative embodiment, in step (2) is in close contact each layer.
In an alternative embodiment, heat treatment described in step (2), temperature be 600~1200 DEG C, soaking time be 60~
180min。
In an alternative embodiment, 600~1200 DEG C are warming up to the heating rate of 1~5 DEG C/min in step (2);It protects
After temperature, 100 DEG C are cooled to the rate of 0.2~0.5 DEG C/min.Rate of temperature fall control may make in adhesive layer glass phase
Thermal stress slow release, prevents adhesive layer from cracking.
The following are several specific embodiments of the invention:
Embodiment 1
The embodiment of the invention provides a kind of silicon nitride fibers of 5 layers of structure to enhance ceramic matric composite, preparation side
Method, comprising:
As shown in Figure 1, preparing the silicon nitride fiber enhancing ceramic matric composite of three kinds of differing dielectric constants respectively, press
According to dielectric constant it is low-in-height-medium-low sequence is combined sequentially into five-layer structure, as shown in Fig. 2, most intermediate high dielectric layer
Dielectric constant is 4.0, and two sides are equal with two layers adjacent of (dielectric layer) dielectric constant of middle layer, is 2.8, two layers of outside is low
The dielectric constant of dielectric layer is equal, is 1.8;The thickness of every layer of five-layer structure is identical, is 3.0mm, and length and width are 120 ×
120mm.The mode that joint face between the layers first passes through spraying spray coating liquor (inorganic wave penetrating paint) in advance coats spray coating liquor
To material surface, inorganic coating quantity for spray is 100g/m2, then the pressure of application 0.5MPa is in close contact five-layer structure.Spray
It is 30wt% that the preparation method of masking liquid, which is in siliconoxide mass content, in the silica solution of purity >=99.9%, be added purity >=
99% yttrium oxide, additional amount account for 20% of siliconoxide mass in silica solution, are dispersed into suspension by ball milling.It keeps applying pressure
While power, layer composite material is heat-treated, spray coating liquor is made to play the role of connection.Heat treatment heating rate is
5 DEG C/min, heat treatment temperature is 1200 DEG C, soaking time 60min, and the rate that 100 DEG C are cooled to after heat preservation is 0.5
℃/min.Finally obtain the five-layer structure composite material having a size of 120 × 120 × 15mm, the X/Ku/Ka of 80% or more transmitance
Band is in 35G or more.
Embodiment 2
The embodiment of the invention provides a kind of silicon nitride fibers of 5 layers of structure to enhance ceramic matric composite, preparation side
Method, comprising:
The mullite fiber enhancing ceramic matric composite for preparing three kinds of differing dielectric constants respectively, according to dielectric constant
It is low-in-height-medium-low sequence is combined sequentially into five-layer structure, the dielectric constant of most intermediate high dielectric layer is 2.8, two sides with
Two layers adjacent of (dielectric layer) dielectric constant of middle layer is equal, is 1.8, the dielectric constant phase of two layers of low dielectric layer in outside
Deng, be 1.2;The thickness of every layer of five-layer structure is identical, is 5.0mm, and length and width are 150 × 150mm.Company between the layers
Silica-based glass phase powder is coated to material surface by the mode that junction first passes through spraying spray coating liquor in advance, and glass phase quantity for spray is
500g/m2, then the pressure of application 0.1MPa is in close contact five-layer structure.The preparation method of spray coating liquor is in silica content
For 60wt%, in the silica solution of purity >=99.9%, the boron oxide powder of purity >=99% is added, by being dispersed with stirring into suspension
Liquid.The additional amount of boron oxide accounts for 5% of silica content in silica solution.It is compound to multilayered structure while keeping applying pressure
Material is heat-treated, and spray coating liquor is made to play the role of connection.Heat treatment heating rate is 2 DEG C/min, heat treatment temperature 800
DEG C, soaking time 120min, the rate that 100 DEG C are cooled to after heat preservation is 0.3 DEG C/min.It finally obtains having a size of 150
The five-layer structure composite material of × 150 × 25mm, the X/Ku/Ka band of 80% or more transmitance is in 45G or more.
Embodiment 3
The embodiment of the invention provides a kind of silicon nitride fibers of 5 layers of structure to enhance ceramic matric composite, preparation side
Method, comprising:
The quartz fibre enhancing ceramic matric composite for preparing three kinds of differing dielectric constants respectively, according to dielectric constant
It is low-in-height-medium-low sequence is combined sequentially into five-layer structure, the dielectric constant of most intermediate high dielectric layer is 3.3, two sides with
Two layers adjacent of (dielectric layer) dielectric constant of middle layer is equal, is 2.3, the dielectric constant phase of two layers of low dielectric layer in outside
Deng, be 1.5;The thickness of every layer of five-layer structure is identical, is 4.2mm, and length and width are 300 × 300mm.Company between the layers
Silica-based glass phase powder is coated to material surface by the mode that junction first passes through spraying spray coating liquor in advance, and glass phase quantity for spray is
250g/m2, then the pressure of application 0.3MPa is in close contact five-layer structure.The preparation method of spray coating liquor is in silica content
For 50wt%, in the silica solution of purity >=99.9%, the alumina powder of purity >=99% is added, by ball milling or is dispersed with stirring
At suspension.The additional amount of aluminium oxide accounts for 10% of silica content in silica solution.While keeping applying pressure, to multilayer knot
Structure composite material is heat-treated, and spray coating liquor is made to play the role of connection.Heat treatment heating rate is 1 DEG C/min, heat treatment temperature
Degree is 600 DEG C, soaking time 60min, and the rate that 100 DEG C are cooled to after heat preservation is 0.2 DEG C/min.Finally obtain size
For the five-layer structure composite material of 300 × 300 × 21mm, the X/Ku/Ka band of 80% or more transmitance is in 40G or more.
The above, optimal specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Content that description in the present invention is not described in detail belongs to professional and technical personnel in the field's well-known technique.
Claims (16)
1. a kind of wideband wave transparent multilayered structure ceramic matric composite, which is characterized in that by the inorganic wave transparent fiber reinforcement of odd-level
Ceramic matric composite is laminated, and the dielectric constant of the inorganic wave transparent fiber reinforced ceramic matrix composites of the odd-level by
Outer layer to middle layer successively increases, and is adhesively fixed between each layer by inorganic wave penetrating paint.
2. wideband wave transparent multilayered structure ceramic matric composite according to claim 1, which is characterized in that inorganic by 5 layers
Wave transparent fiber reinforced ceramic matrix composites is laminated, and inter level dielectric constant is 2.8~4.0, with the middle layer phase
Adjacent two layers of dielectric constant is 1.8~2.8, and outermost two layers of dielectric constant is 1.2~1.8.
3. wideband wave transparent multilayered structure ceramic matric composite according to claim 1, which is characterized in that described inorganic
Wave coating is that inorganic wave transparent ceramic powder is dispersed in the suspension formed in silica solution.
4. wideband wave transparent multilayered structure ceramic matric composite according to claim 3, which is characterized in that described inorganic
Wave ceramic powder is at least one of boron oxide, aluminium oxide, yttrium oxide, silicon nitride or boron nitride powder.
5. wideband wave transparent multilayered structure ceramic matric composite according to claim 3 or 4, which is characterized in that the silicon
Purity >=99.9% of colloidal sol, the mass content of silica are 30~60%;The purity of the inorganic wave transparent ceramic powder >=
99%, the quality of the inorganic wave transparent ceramic powder is the 5%~20% of the siliconoxide mass.
6. the wideband wave transparent multilayered structure ceramic matric composite according to claim, which is characterized in that each thickness degree is equal
For 3.0~5.0mm.
7. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite, which comprises the following steps:
(1) the inorganic wave transparent fiber reinforced ceramic matrix composites of odd-level is successively increased according to dielectric constant by outer layer to middle layer
The sequence added stacks, and inorganic wave penetrating paint is applied between adjacent two layers before stacking;
(2) applying pressure is in close contact each layer, is heat-treated, obtains multilayered structure ceramic matric composite.
8. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 7, feature
Be, 5 layers of inorganic wave transparent fiber reinforced ceramic matrix composites be laminated in step (1), and inter level dielectric constant be 2.8~
4.0, the dielectric constant with the middle layer adjacent two layers is 1.8~2.8, and outermost two layers of dielectric constant is 1.2~1.8.
9. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 7, feature
It is, step (1) the inorganic wave penetrating paint is that inorganic wave transparent ceramic powder is dispersed in the suspension formed in silica solution.
10. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 9, feature
It is, the inorganic wave transparent ceramic powder is at least one in boron oxide, aluminium oxide, yttrium oxide, silicon nitride or boron nitride powder
Kind.
11. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 9 or 10,
It is characterized in that, purity >=99.9% of the silica solution, the mass content of silica is 30~60%;The inorganic wave transparent ceramics
Purity >=99% of powder, the quality of the inorganic wave transparent ceramic powder are the 5%~20% of the siliconoxide mass.
12. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 11, special
Sign is, is applied by the way of spraying to the inorganic wave penetrating paint, and quantity for spray is 100~500g/m2。
13. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 7, feature
It is, each thickness degree is 3.0~5.0mm in step (1).
14. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 7, feature
It is, applying 0.1~0.5MPa pressure in step (2) is in close contact each layer.
15. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 7, feature
It is, heat treatment described in step (2), temperature is 600~1200 DEG C, and soaking time is 60~180min.
16. a kind of preparation method of wideband wave transparent multilayered structure ceramic matric composite according to claim 15, special
Sign is, is warming up to 600~1200 DEG C in step (2) with the heating rate of 1~5 DEG C/min;After heat preservation, with 0.2~0.5
DEG C/rate of min is cooled to 100 DEG C.
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Cited By (2)
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CN113735598A (en) * | 2021-08-05 | 2021-12-03 | 西安交通大学 | High-strength high-temperature-ablation-resistant high-wave-transmission silicon nitride-based composite ceramic and preparation method thereof |
CN114057503A (en) * | 2021-12-14 | 2022-02-18 | 航天特种材料及工艺技术研究所 | Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof |
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CN113735598A (en) * | 2021-08-05 | 2021-12-03 | 西安交通大学 | High-strength high-temperature-ablation-resistant high-wave-transmission silicon nitride-based composite ceramic and preparation method thereof |
CN113735598B (en) * | 2021-08-05 | 2022-10-28 | 西安交通大学 | High-strength high-temperature-ablation-resistant high-wave-transmission silicon nitride-based composite ceramic and preparation method thereof |
CN114057503A (en) * | 2021-12-14 | 2022-02-18 | 航天特种材料及工艺技术研究所 | Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof |
CN114057503B (en) * | 2021-12-14 | 2022-09-02 | 航天特种材料及工艺技术研究所 | Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof |
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