CN114057503A - Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof - Google Patents

Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof Download PDF

Info

Publication number
CN114057503A
CN114057503A CN202111523554.6A CN202111523554A CN114057503A CN 114057503 A CN114057503 A CN 114057503A CN 202111523554 A CN202111523554 A CN 202111523554A CN 114057503 A CN114057503 A CN 114057503A
Authority
CN
China
Prior art keywords
density gradient
fabric
density
gradient
composite material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111523554.6A
Other languages
Chinese (zh)
Other versions
CN114057503B (en
Inventor
吴焘
苑贺楠
李阳
杨小波
张剑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Aerospace Research Institute of Materials and Processing Technology
Original Assignee
Aerospace Research Institute of Materials and Processing Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aerospace Research Institute of Materials and Processing Technology filed Critical Aerospace Research Institute of Materials and Processing Technology
Priority to CN202111523554.6A priority Critical patent/CN114057503B/en
Publication of CN114057503A publication Critical patent/CN114057503A/en
Application granted granted Critical
Publication of CN114057503B publication Critical patent/CN114057503B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/14—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 silica
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C04B2235/775—Products showing a density-gradient

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention relates to a density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and a preparation method thereof. The method comprises the following steps: (1) preparing a density gradient fabric with gradually increased fiber volume density from top to bottom along the thickness direction by adopting quartz fibers; (2) adopting silica sol to dip the density gradient fabric, and then carrying out gradient drying; the gradient drying comprises the following steps: wrapping and sealing the upper surface and the side surface of the density gradient fabric by using a film, and then flatly placing the fabric on a metal net of an oven for blast drying; (3) repeating the step (2) at least once to obtain a composite material blank; (4) and carrying out high-temperature treatment on the composite material blank to obtain the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite. The method develops a new method for preparing the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material by superposing the dual gradient effects of the density gradient fabric and the gradient drying process.

Description

Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a density gradient quartz fiber reinforced silica ceramic matrix composite material and a preparation method thereof.
Background
The quartz fiber reinforced silica composite material is a ceramic-based wave-transmitting material which is relatively mature in domestic application, has good high-temperature wave-transmitting performance and mechanical property, is commonly used for antenna housing and antenna window products, and can also be simply used as a bearing heat-insulating structural member. The density of the existing quartz fiber reinforced silicon dioxide composite material is uniform, the material often has temperature gradient distribution along the thickness direction in the using process, the thermal stress exists in the material, and the density gradient material can effectively relieve the thermal stress in the material. On the other hand, the dielectric constant of the composite material is directly related to the density, the density gradient material is also the dielectric gradient material, and through reasonable design, the density gradient material can expand the wave-transmitting frequency bandwidth of the product. Due to the difficulty of the process preparation, the preparation method of the density gradient quartz fiber reinforced silicon dioxide composite material is still limited at present, and only a few reports exist. Chinese patent application CN109293385A discloses co-weaving organic fibers in a flat quartz fiber fabric, the content of the organic fibers shows gradient change along the thickness direction, removing the organic fibers by high temperature sintering after composite impregnation, and regulating the density of the material along the thickness direction to obtain a density gradient material. However, this method is liable to cause problems such as incomplete thermal decomposition of the organic fibers and remaining of continuous voids after the decomposition.
In view of the above, there is a need for a new density gradient silica ceramic matrix composite and a method for preparing the same.
Disclosure of Invention
The invention aims to overcome the defects of the existing preparation method of the density gradient quartz fiber reinforced silica ceramic matrix composite material, and realizes the efficient preparation of the density gradient quartz fiber reinforced silica ceramic matrix composite material only by optimizing the structure of the fabric and the drying process.
The invention provides a preparation method of a density gradient quartz fiber reinforced silica ceramic matrix composite material in a first aspect, which comprises the following steps:
(1) preparing a density gradient fabric with gradually increased fiber volume density from top to bottom along the thickness direction by adopting quartz fibers;
(2) adopting silica sol to dip the density gradient fabric, and then carrying out gradient drying; the gradient drying comprises the following steps: wrapping and sealing the upper surface and the side surface of the density gradient fabric by using a film, and then flatly placing the fabric on a metal net of an oven for blast drying;
(3) repeating the step (2) at least once to obtain a composite material blank;
(4) and carrying out high-temperature treatment on the composite material blank to obtain the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite.
Preferably, the fiber volume density of the density gradient fabric is 0.2-1.1 g/cm in the thickness direction3Is tapered within a range of (1).
Preferably, the solid content of the silica sol is 20-25%.
Preferably, the impregnation is: and vacuum dipping the density gradient fabric for 24-72 hours by adopting the silica sol.
Preferably, step (2) is repeated no more than 5 times.
Preferably, the temperature of the high-temperature treatment is 500-800 ℃, and the time of the high-temperature treatment is 1-2 h.
Preferably, the temperature for air blast drying is 50-80 ℃, and the time for air blast drying is 3-4 h.
Preferably, the film is a plastic film, preferably a cling film.
Preferably, the density gradient fabric is a flat fabric, the flat fabric has 3-8 incremental fiber volume density values from top to bottom along the thickness direction, and the thickness of the fabric corresponding to each fiber volume density value is 2-10 mm.
In a second aspect, the present invention provides a density gradient silica fiber reinforced ceramic matrix composite prepared by the method of the first aspect of the present invention.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the invention, the density gradient of the prefabricated fabric and the density gradient spontaneously formed by the glue solution in the gradient drying process are superposed to realize the efficient preparation of the density gradient quartz fiber reinforced silica ceramic-based composite material, so that the problems of incomplete thermal decomposition and continuity defect introduced in the organic fiber sintering process in the existing density gradient quartz fiber reinforced silica ceramic-based composite material can be effectively avoided.
(2) In the gradient drying process, the lower layer with high fiber volume content of the density gradient fabric is in direct contact with the outside, the drying is fastest, and the density of the lower layer silica sol is increased due to water loss; and because only the lower surface of the density gradient fabric is a drying channel, under the capillary action, the silica sol on the upper layer of the fabric tends to migrate downwards, so that the density of the silica sol in the fabric is gradually increased from top to bottom; the invention discovers that the superposition of the density gradient of the glue solution and the density gradient of the fabric can enable the final material to present obvious density gradient in the thickness direction from top to bottom, realize obvious gradient effect of dielectric, and further improve the broadband wave-transmitting performance greatly compared with the material with uniform density.
(3) The method develops a new method for preparing the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material by superposing the dual gradient effects of the density gradient fabric and the gradient drying process.
(4) The method has the advantages of simple operation, low cost and high preparation efficiency, and is favorable for preparing the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material with remarkable density gradient.
Drawings
FIG. 1 is a flow chart of the manufacturing process of the present invention. In FIG. 1, the density gradient silica ceramic matrix composite is abbreviated as a density gradient composite.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a preparation method of a density gradient quartz fiber reinforced silica ceramic matrix composite material in a first aspect, which comprises the following steps:
(1) preparing a density gradient fabric (also called as a density gradient preform fabric) with gradually increased fiber volume density from top to bottom along the thickness direction by adopting quartz fibers; in the present invention, it is preferable that the density gradient fabric is a flat fabric;
(2) adopting silica sol to dip the density gradient fabric, and then carrying out gradient drying; the gradient drying comprises the following steps: wrapping and sealing the upper surface and the side surfaces (periphery) of the density gradient fabric by using a film (such as a plastic film), and then flatly placing the fabric on a metal net of an oven for blast drying, wherein the lower surface of the density gradient fabric is directly exposed to the air in the blast drying process; specifically, the upper surface and the side surfaces (periphery) of the density gradient fabric are wrapped and sealed by plastic films (preferably preservative films), namely the lower surface of the density gradient fabric is removed, and the other surfaces are wrapped and sealed by the plastic films; when the fabric is dried by air blowing, the fabric is flatly placed on a metal net (such as a stainless steel net) of an oven, the metal net in the oven and the bottom surface of the oven have a certain height, so that the lower surface (lower bottom surface) of the density gradient fabric can be directly and fully exposed in the air, and the fabric is dried by air blowing in the oven at 50-80 ℃;
(3) repeating the step (2) at least once to obtain a composite material blank;
(4) and carrying out high-temperature treatment on the composite material blank to obtain the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite.
In the gradient drying process, the lower layer (lower surface) with high fiber volume content of the density gradient fabric is in direct contact with the outside, the drying is fastest, and the density of the lower layer of silica sol is increased due to water loss; and because only the lower surface of the density gradient fabric is a drying channel, under the capillary action, the silica sol on the upper layer of the fabric tends to migrate downwards, so that the density of the silica sol in the fabric is gradually increased from top to bottom; the invention discovers that the superposition of the density gradient of the glue solution and the density gradient of the fabric can enable the final material to present obvious density gradient in the thickness direction from top to bottom, realize obvious gradient effect of dielectric, and further improve the broadband wave-transmitting performance greatly compared with the material with uniform density.
According to the invention, the density gradient of the prefabricated fabric and the density gradient spontaneously formed by the glue solution in the gradient drying process are superposed to realize the efficient preparation of the density gradient quartz fiber reinforced silica ceramic-based composite material, so that the problems of incomplete thermal decomposition and continuity defect introduced in the organic fiber sintering process in the existing density gradient quartz fiber reinforced silica ceramic-based composite material can be effectively avoided.
According to some preferred embodiments, the fiber volume density of the density gradient fabric is 0.2 to 1.1g/cm from top to bottom in the thickness direction3Is graded (gradual).
According to some preferred embodiments, the silica sol has a solid content of 20 to 25%; in the present invention, the silica sol may be, for example, a commercially available industrial-grade silica sol having a solid content of 20 to 25%.
According to some preferred embodiments, the impregnation is vacuum impregnation.
According to some preferred embodiments, the impregnation is: vacuum-dipping the density gradient fabric for 24-72 h (for example, 24, 36, 48, 60 or 72h) by using the silica sol; specifically, for example, under the condition of vacuum pumping (preferably, the relative vacuum degree is lower than-0.09 MPa), the silica sol is filled in a closed container in which the density gradient fabric is placed, and the density gradient fabric is taken out after vacuum impregnation is carried out for 24-72 hours.
According to some preferred embodiments, the number of times step (2) is repeatedNot more than 5 times; in the invention, the density of the whole material can be increased by repeating the step (2) and increasing the times of impregnation (composite impregnation), the specific times of impregnation are adjusted according to the actually required density, but the total times of impregnation are preferably controlled within 5 times, because the density of the lower layer of the density gradient fabric after 5 times of impregnation is close to 1.70g/cm3If the density of the lower layer is difficult to be further increased by continuous impregnation, the density of the upper layer material is still low at this time, and the upper layer material has the potential of continuous weight increment, so that the problem that the density difference between the upper layer and the lower layer tends to be reduced is easily caused.
According to some preferred embodiments, the high-temperature treatment is performed at a temperature of 500 to 800 ℃ (e.g., 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, or 800 ℃), for a time of 1 to 2 hours, and the high-temperature treatment atmosphere is an air atmosphere.
According to some preferred embodiments, the temperature for forced air drying is 50 to 80 ℃ (e.g., 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃), and the time for forced air drying is, e.g., 3 to 4 hours; in some embodiments, the particular air drying time may be sufficient to ensure that the moisture of the matte is evaporated.
According to some preferred embodiments, the film is a plastic film, preferably a cling film; the wrap film may be, for example, a commercially available wrap film directly available.
According to some preferred embodiments, the density gradient fabric is a flat fabric having 3 to 8 (e.g., 3, 4, 5, 6, 7, or 8) increasing fiber bulk density values from top to bottom in the thickness direction, each fiber bulk density value corresponding to a fabric thickness of 2 to 10mm (e.g., 2, 3, 4, 5, 6, 7, 8, 9, or 10 mm).
In a second aspect, the present invention provides a density gradient silica fiber reinforced ceramic matrix composite prepared by the method of the first aspect of the present invention.
The invention will be further illustrated by way of example, but the scope of protection is not limited to these examples. The present invention is capable of other embodiments, and various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Example 1
The method is characterized in that a commercially available 190tex B-type quartz fiber and a commercially available silica hydrosol (silica sol) with the solid content of 20-25% are adopted as raw materials to prepare the density gradient quartz fiber reinforced silica ceramic matrix composite, and the method is realized by the following steps:
weaving density gradient fabric (density gradient flat fabric), wherein the fiber volume density is 0.2g/cm from top to bottom along the thickness direction3，0.4g/cm3，0.6g/cm3The weave thickness for each fiber bulk density is 5 mm.
Secondly, under the condition of vacuum pumping, the silica sol is filled in a closed container with the density gradient fabric, and the density gradient fabric is taken out after being soaked for 48 hours. Wrapping and sealing the upper surface and the periphery (side face) of the soaked density gradient fabric by using a preservative film, placing the density gradient fabric wrapped with the preservative film on a stainless steel net of an oven, directly exposing the lower surface of the density gradient fabric to the air, and carrying out forced air drying at 50 ℃ in the oven for 4 hours.
And thirdly, repeating the step two for 4 times to obtain the final composite material blank.
Fourthly, the composite material blank obtained in the third step is processed for 1 hour at the high temperature of 600 ℃ in the air atmosphere, and the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material is obtained.
The density of the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the embodiment is tested by sampling every 5mm in the thickness direction, and the density is 0.63g/cm from top to bottom in sequence3，1.15g/cm3，1.48g/cm3The density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the embodiment has a remarkable density gradient, and the difference between every two adjacent density values is 0.33g/cm3Above, its density gradient characteristics are even better than the original onesThe density gradient characteristics of the density gradient fabric are more pronounced.
The dielectric constants of the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared in the embodiment were sampled every 5mm in the thickness direction, and the dielectric constants were 1.5, 2.3, and 2.7 in order from top to bottom.
The density gradient quartz fiber reinforced silica ceramic matrix composite flat plate prepared by the embodiment is subjected to a wave transmission performance test, and the frequency band bandwidth with the transmittance of more than 80% can reach more than 8 GHz.
Example 2
The method is characterized in that a commercially available 190tex B-type quartz fiber and a commercially available silica hydrosol (silica sol) with the solid content of 20-25% are adopted as raw materials to prepare the density gradient quartz fiber reinforced silica ceramic matrix composite, and the method is realized by the following steps:
weaving density gradient fabric (density gradient flat fabric), wherein the fiber volume density is 0.2g/cm from top to bottom along the thickness direction of the flat fabric3，0.4g/cm3，0.6g/cm3，0.75g/cm3，1g/cm3The weave thickness for each fiber bulk density is 5 mm.
Secondly, under the condition of vacuum pumping, the silica sol is filled in a closed container with the density gradient fabric, and the density gradient fabric is taken out after being soaked for 48 hours. Wrapping and sealing the upper surface and the periphery (side face) of the soaked density gradient fabric by using a preservative film, placing the density gradient fabric wrapped with the preservative film on a stainless steel net of an oven, directly exposing the lower surface of the density gradient fabric to the air, and carrying out forced air drying at 50 ℃ in the oven for 4 hours.
And thirdly, repeating the step two for 4 times to obtain the final composite material blank.
Fourthly, the composite material blank obtained in the third step is processed for 1 hour at the high temperature of 600 ℃ in the air atmosphere, and the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material is obtained.
The density of the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the embodiment is tested by sampling every 5mm in the thickness direction, and the density is measured from the topThe density is 0.65g/cm in sequence from bottom to top3，0.95g/cm3，1.25g/cm3，1.45g/cm3，1.71g/cm3. The density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the embodiment has a remarkable density gradient, and the density gradient characteristic is even more remarkable than that of the original density gradient fabric.
The dielectric constants of the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared in the embodiment were sampled every 5mm in the thickness direction, and the dielectric constants were 1.55, 1.9, 2.35, 2.6, and 3.2 in order from top to bottom.
The density gradient quartz fiber reinforced silica ceramic matrix composite flat plate prepared by the embodiment is subjected to a wave transmission performance test, and the frequency band bandwidth with the transmittance of more than 80% can reach more than 10 GHz.
Comparative example 1
The method is characterized in that a commercially available 190tex B-type quartz fiber and a commercially available silica hydrosol (silica sol) with the solid content of 20-25% are adopted as raw materials to prepare the density gradient quartz fiber reinforced silica ceramic matrix composite, and the method is realized by the following steps:
weaving density gradient fabric (density gradient flat fabric), wherein the fiber volume density is 0.2g/cm from top to bottom along the thickness direction3，0.4g/cm3，0.6g/cm3The weave thickness for each fiber bulk density is 5 mm.
Secondly, under the condition of vacuum pumping, the silica sol is filled in a closed container in which the density gradient fabric is placed, the density gradient fabric is taken out after being soaked for 48 hours, and the soaked density gradient fabric is directly dried by air blowing for 4 hours at 50 ℃ in a drying oven.
And thirdly, repeating the step two for 4 times to obtain the final composite material blank.
Fourthly, the composite material blank obtained in the third step is processed for 1 hour at the high temperature of 600 ℃ in the air atmosphere, and the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material is obtained.
The density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite prepared by the comparative exampleThe material is sampled every 5mm in the thickness direction to test the material density, and the density is 1.36g/cm from top to bottom in sequence3，1.41g/cm3，1.47g/cm3. The comparative example does not adopt a gradient drying process, and the density gradient characteristic of the density gradient quartz fiber reinforced silica ceramic matrix composite prepared by the comparative example is not obvious compared with the original density gradient fabric.
The dielectric constants of the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the comparative example are tested by sampling every 5mm in the thickness direction, and are 2.5, 2.55 and 2.65 from top to bottom.
And (3) carrying out a wave-transparent performance test on the density gradient quartz fiber reinforced silica ceramic matrix composite plate prepared by the comparative example, and measuring that the frequency band bandwidth with the transmittance of more than 80% is not more than 6 GHz.
Comparative example 2
The method is characterized in that a commercially available 190tex B-type quartz fiber and a commercially available silica hydrosol (silica sol) with the solid content of 20-25% are adopted as raw materials to prepare the density gradient quartz fiber reinforced silica ceramic matrix composite, and the method is realized by the following steps:
weaving flat fabric with uniform density, wherein the fiber volume density is 0.6g/cm3And the thickness is 15 mm.
Secondly, under the condition of vacuum pumping, the silica sol is filled in a closed container in which the flat fabric with uniform density is placed, and the flat fabric with uniform density is taken out after being soaked for 48 hours. Wrapping and sealing the upper surface and the periphery (side face) of the soaked flat fabric with uniform density by using a preservative film, placing the flat fabric with uniform density wrapped with the preservative film on a stainless steel net of an oven, directly exposing the lower surface of the flat fabric with uniform density to the air, and carrying out forced air drying for 4 hours at 50 ℃ in the oven.
And thirdly, repeating the step two for 4 times to obtain the final composite material blank.
Fourthly, the composite material blank obtained in the third step is processed for 1 hour at the high temperature of 600 ℃ in the air atmosphere, and the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material is obtained.
The density of the material is tested by sampling the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the comparative example every 5mm in the thickness direction, and the density is 1.30g/cm from top to bottom in sequence3，1.38g/cm3，1.47g/cm3. Although the density gradient composite material can be obtained by adopting the flat fabric with uniform density and combining the gradient drying process, the density gradient characteristic of the material is not obvious compared with the density gradient quartz fiber reinforced ceramic matrix composite material prepared by adopting the density gradient fabric.
The dielectric constants of the density gradient quartz fiber reinforced silica ceramic matrix composite material prepared by the comparative example are tested by sampling every 5mm in the thickness direction, and are 2.4, 2.52 and 2.65 from top to bottom.
And (3) carrying out a wave-transparent performance test on the density gradient quartz fiber reinforced silica ceramic matrix composite plate prepared by the comparative example, and measuring that the frequency band bandwidth with the transmittance of more than 80% is not more than 6 GHz.
According to the embodiment and the comparative example of the invention, the density gradient quartz fiber reinforced silica ceramic matrix composite material with obvious density gradient is prepared by superposing the dual gradient effect of the density gradient fabric and the gradient drying process, and the density difference of the upper surface and the lower surface of the prepared density gradient quartz fiber reinforced silica ceramic matrix composite material reaches 0.85g/cm3As described above, when the silica ceramic matrix composite is prepared by using only the density gradient fabric or only the gradient drying process, although the density gradient composite can be obtained, the density gradient characteristics of the material are not obvious, and the difference between the densities of the upper and lower surfaces of the prepared material is not more than 0.2g/cm3。
The invention has not been described in detail and is in part known to those of skill in the art.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation method of a density gradient quartz fiber reinforced silica ceramic matrix composite is characterized by comprising the following steps:
(1) preparing a density gradient fabric with gradually increased fiber volume density from top to bottom along the thickness direction by adopting quartz fibers;
(2) adopting silica sol to dip the density gradient fabric, and then carrying out gradient drying; the gradient drying comprises the following steps: wrapping and sealing the upper surface and the side surface of the density gradient fabric by using a film, and then flatly placing the fabric on a metal net of an oven for blast drying;
(3) repeating the step (2) at least once to obtain a composite material blank;
(4) and carrying out high-temperature treatment on the composite material blank to obtain the density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite.
2. The method of claim 1, wherein:
the fiber volume density of the density gradient fabric is 0.2-1.1 g/cm in the thickness direction3Is tapered within a range of (1).
3. The method of claim 1, wherein:
the solid content of the silica sol is 20-25%.
4. The method of claim 1, wherein:
the impregnation is as follows: and vacuum dipping the density gradient fabric for 24-72 hours by adopting the silica sol.
5. The method of claim 1, wherein:
the number of times of repeating the step (2) is not more than 5.
6. The method of claim 1, wherein:
the temperature of the high-temperature treatment is 500-800 ℃, and the time of the high-temperature treatment is 1-2 h.
7. The production method according to any one of claims 1 to 6, characterized in that:
the temperature for carrying out the forced air drying is 50-80 ℃, and the time for carrying out the forced air drying is 3-4 h.
8. The production method according to any one of claims 1 to 6, characterized in that:
the film is a plastic film, preferably a preservative film.
9. The production method according to any one of claims 1 to 6, characterized in that:
the density gradient fabric is a flat fabric, the flat fabric has 3-8 fiber volume density values which are gradually increased from top to bottom along the thickness direction, and the thickness of the fabric corresponding to each fiber volume density value is 2-10 mm.
10. A density gradient silica fiber reinforced ceramic matrix composite produced by the production method according to any one of claims 1 to 9.
CN202111523554.6A 2021-12-14 2021-12-14 Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof Active CN114057503B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111523554.6A CN114057503B (en) 2021-12-14 2021-12-14 Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111523554.6A CN114057503B (en) 2021-12-14 2021-12-14 Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114057503A true CN114057503A (en) 2022-02-18
CN114057503B CN114057503B (en) 2022-09-02

Family

ID=80229369

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111523554.6A Active CN114057503B (en) 2021-12-14 2021-12-14 Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114057503B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998009811A1 (en) * 1996-09-05 1998-03-12 C.T.M.I. Cotton Textiles Pour Materiaux Innovants Composite ceramic material with sandwich type structure
CN103601479A (en) * 2013-11-14 2014-02-26 山东工业陶瓷研究设计院有限公司 Preparation method for high-temperature-resistant ultra-thin antenna window
CN113348748B (en) * 2011-10-14 2014-03-19 山东工业陶瓷研究设计院有限公司 Quartz fiber reinforced quartz ceramic matrix composite material and preparation method thereof
CN104446584A (en) * 2014-11-03 2015-03-25 湖北三江航天江北机械工程有限公司 Moulding method of variable-density broadband wave-transparent quartz composite ceramic antenna housing body
CN109400194A (en) * 2018-10-30 2019-03-01 山东工业陶瓷研究设计院有限公司 The compound composite antenna housing of W-waveband fiber reinforced ceramic-base and preparation method
CN109664568A (en) * 2019-01-23 2019-04-23 航天材料及工艺研究所 A kind of wideband wave transparent multilayered structure ceramic matric composite and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998009811A1 (en) * 1996-09-05 1998-03-12 C.T.M.I. Cotton Textiles Pour Materiaux Innovants Composite ceramic material with sandwich type structure
EP0925179A1 (en) * 1996-09-05 1999-06-30 C.T.M.I. Cotton Textiles Pour Materiaux Innovants Composite ceramic material with sandwich type structure
CN113348748B (en) * 2011-10-14 2014-03-19 山东工业陶瓷研究设计院有限公司 Quartz fiber reinforced quartz ceramic matrix composite material and preparation method thereof
CN103601479A (en) * 2013-11-14 2014-02-26 山东工业陶瓷研究设计院有限公司 Preparation method for high-temperature-resistant ultra-thin antenna window
CN104446584A (en) * 2014-11-03 2015-03-25 湖北三江航天江北机械工程有限公司 Moulding method of variable-density broadband wave-transparent quartz composite ceramic antenna housing body
CN109400194A (en) * 2018-10-30 2019-03-01 山东工业陶瓷研究设计院有限公司 The compound composite antenna housing of W-waveband fiber reinforced ceramic-base and preparation method
CN109664568A (en) * 2019-01-23 2019-04-23 航天材料及工艺研究所 A kind of wideband wave transparent multilayered structure ceramic matric composite and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
韩爽等: "2.5D SiO_(2f)/SiO_2复合材料制备工艺及性能研究", 《稀有金属材料与工程》 *
高龙飞等: "连续石英纤维增强二氧化硅复合材料研究概况", 《玻璃钢/复合材料》 *

Also Published As

Publication number Publication date
CN114057503B (en) 2022-09-02

Similar Documents

Publication Publication Date Title
CN114057503B (en) Density gradient quartz fiber reinforced silicon dioxide ceramic matrix composite material and preparation method thereof
CN1229221C (en) Vacuum insualtor using glass white wool and its fabrication method
US2970936A (en) Insulated electrical coils
JPH083464A (en) Synthesized ferroelectric aerogel for variable-voltage dielectric tuning and its production
CN111662678B (en) High-temperature antioxidant flexible graphite filler, preparation method and high-temperature antioxidant flexible graphite packing
CN104494027B (en) Double vacuum bag microwave solidification methods of carbon fibre composite product
CN109180194A (en) A kind of compound density method of the different conditions polymer infiltration and pyrolysis of SiC based composites
CN112592152A (en) Porcelain cross arm insulator and manufacturing method thereof
CN108623296A (en) A kind of wet-method extrusion manufacturing method of soft magnetic ferrite
CN105199297A (en) Bismaleimide resin premix with good dielectric property as well as preparation method and device of bismaleimide resin premix
CN110394994A (en) A kind of moulding technique of semi-solid preparation mica products foil
FI76781C (en) Process for sealing porous structural members of a non-oxidizing ceramic raw material for hot isostatic pressing
Zhou et al. Influence of sintering process on the microwave dielectric properties of Bi (V0. 008Nb0. 992) O4 ceramics
CN114414045A (en) Calibration method of solar radiometer
CN106262793A (en) A kind of preparation method keeping original color shape flavor mushroom dry
CN111807722A (en) Functional gas for hollow glass spacing layer
CN111960821A (en) Microwave dielectric ceramic material and preparation method and application thereof
McRae et al. Intercalation compound resistivity measurements
CN108341588A (en) A kind of preparation method of high-compactness silica crucible
Nguyen‐Tuong Vacuum outgassing of artificial dielectric ceramics
US6939493B2 (en) Method for the production of composite materials
CN212603544U (en) Equipment for manufacturing insulating rod
CN114988877B (en) Ultralow-loss microwave dielectric ceramic material and preparation method thereof
CN103387417A (en) Dampproof method for porous ceramic material containing silicon hydroxyl
CN1104232A (en) Composite sealing material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant