CN110511008A - High-compactness quartz/quartz composite material and preparation method based on freeze drying process - Google Patents
High-compactness quartz/quartz composite material and preparation method based on freeze drying process Download PDFInfo
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- CN110511008A CN110511008A CN201910925391.0A CN201910925391A CN110511008A CN 110511008 A CN110511008 A CN 110511008A CN 201910925391 A CN201910925391 A CN 201910925391A CN 110511008 A CN110511008 A CN 110511008A
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q1/00—Details of, or arrangements associated with, antennas
- H01Q1/42—Housings not intimately mechanically associated with radiating elements, e.g. radome
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
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Abstract
The present invention discloses a kind of high-compactness quartz/quartz composite material and preparation method based on freeze drying process, the preparation method first pre-processes silica fibrage object, then the silicon sol solution vacuum impregnation and freeze drying process process of multiple different-grain diameter solute are carried out respectively to silica fibrage object, silica substrate is obtained finally by sintering processes, finally obtains quartz/quartz composite material.Preparation method preparation process provided by the invention is simple, manufacturing cycle is obviously shortened, is at low cost, and the composite property being prepared is excellent；Composite material consistency provided by the invention is high, density gradient is small, excellent in mechanical performance, can be applied to antenna house, antenna windows and other aerospace fields.
Description
Technical field
The present invention relates to technology field of ceramic matrix composite material, especially a kind of high-compactness based on freeze drying process
Quartz/quartz composite material and preparation method.
Background technique
It is a kind of to have heat-insulated wave transparent, higher that quartz fibre, which enhances quartzy composite material (quartz/quartz composite material),
The composite material of mechanical strength and a series of excellent comprehensive performances such as lower dielectric constant and loss, impact resistance, in high temperature
Electromagnetic wave transparent material field has a wide range of applications, and is one of the ideal chose for making radar antenna cover material.
The preparation method of quartz/quartz composite material mainly includes hot pressed sintering, chemical vapor infiltration, sol-gel etc.
Technique.Heat pressing process requires high and demoulding difficult agglomerating plant, further, since hot pressed sintering temperature is higher, quartz fibre analysis
It is brilliant serious, composite property decline.It is complicated, heavy that chemical vapor infiltration technique prepares quartz/quartz composite technology process
The product process time is long, preparation cost is higher.Currently, the most mature preparation process of quartz/quartz composite material is sol-gel work
Skill, the basic process of the technique is that quartz textile is put into silica solution to impregnate, and by drying and dehydrating, colloidal sol becomes solidifying
Glue finally sinters quartz/quartz composite material into.The major advantage of sol-gel technology is that sintering temperature is low, fibre damage phase
To smaller, it can be achieved that dead size molding, the disadvantage is that SiO 2-ceramic yield is lower, needs molten by repeated multiple times dipping silicon
It is prepared by glue and gelation and sintering process.Since silicon sol solution mass fraction is generally lower, and pickling efficiency is low, and use is molten
When glue-gel process method prepares quartz/quartz composite material, densifying materials usually require more than ten or even tens dippings
With gel drying process, material long preparation period, cost are big.Particularly, after repeatedly densifying dipping, silica solution is difficult to lead to
It crosses and is impregnated into composite inner hole again, especially for the silica fibrage object of Hou Du≤40mm, so that material
Density is difficult to improve, and leads to composite material there are consistency the disadvantages of low, density gradient is big, mechanical property is insufficient.
Summary of the invention
The present invention provides a kind of high-compactness quartz/quartz composite material based on freeze drying process and its preparation side
Method, for overcoming defect in the prior art, by first using bulky grain silicon sol solution dipping+freeze drying process, then with small
Particle silicon sol solution dipping+freeze drying process preparation method makes composite material consistency height, the density level bands being prepared
Small, excellent in mechanical performance is spent, and preparation process is simple, manufacturing cycle is obviously shortened, is at low cost.
To achieve the above object, the present invention proposes that a kind of high-compactness quartz/quartz based on freeze drying process is compound
Material, the composite material is using silica fibrage object as reinforced phase, using silica as matrix；It is quartzy in the composite material
The volume fraction of fibrous braid is 40~47%；The composite material can be applied to antenna house, antenna windows and other aviations boat
Its field.
To achieve the above object, the present invention also proposes that a kind of high-compactness quartz/quartz based on freeze drying process is multiple
Condensation material preparation method, comprising the following steps:
S1: silica fibrage object is placed in immersion treatment in organic solvent, is dried；
S2: vacuum impregnation will be carried out by the silica fibrage object of step S1, freeze-drying work is carried out after the completion of dipping
Skill repeats the vacuum impregnation and freeze drying process process 3~4 times；The vacuum-impregnated impregnating agent is that solute partial size is
The silicon sol solution of 40~50nm；
S3: vacuum impregnation and freeze drying process process 2~3 will be continued by the silica fibrage object of step S2
It is secondary；The vacuum-impregnated impregnating agent is the silicon sol solution that solute partial size is 10~20nm；
S4: final to obtain by being sintered by the silica fibrage object of step S3 to obtain silica substrate
To quartz/quartz composite material.
Compared with prior art, the beneficial effects of the present invention are as follows:
1, the high-compactness quartz/quartz composite material and preparation method thereof provided by the invention based on freeze drying process, it is first
Immersion treatment first is carried out to silica fibrage object, with impurity such as the dust, the sizes that remove fiber surface；Then to quartzy fine
Dimension braided fabric carries out the silicon sol solution vacuum impregnation and freeze drying process process of multiple different-grain diameter solute respectively, finally leads to
Oversintering handles to obtain silica substrate, finally obtains quartz/quartz composite material.Preparation method provided by the invention, base
In dipping process early period, silica fibrage object impregnation channel size is micron dimension, in order to improve dipping efficiency of densification,
Preceding 3~4 dippings select the silicon sol solution dipping of big partial size (40~50nm) solute, and subsequent 2~3 times using ultra-small grain size
The silicon sol solution of (10~20nm) solute is impregnated, and it is compound to complete densification.Solute partial size selects in silica solution maceration extract
Principle be it is descending, successively impregnate, first select big partial size silica solution fiberfill fibers braided part overall skeleton, then pass through small particle
The dipping of silica solution is sufficient filling with material hole, keeps material full densificationization compound.Meanwhile the present invention uses freeze drying process
Silica fibrage object after dipping is dried, by the drying process, material is in the drying process due to by freezing
It is fixed, make under conditions of low-temperature high-vacuum the moisture in sample directly distilled by ice achieve the purpose that it is dry, in dry mistake
Not by the effect of surface tension in journey, the product of preparation is indeformable, and volume is almost unchanged, can keep original structure well,
Material is in penetrating porous structure after drying, and silica solution enters material internal, packing material hole, Neng Gou when convenient for impregnating again
Densifying materials degree is further increased while reducing density of material gradient, high-compactness quartz/stone of even density is made
English composite material.It is preparation method simple process provided by the invention, short preparation period, at low cost, it can be used for Hou Du≤40mm's
The preparation of fiber-reinforcement silicon dioxide ceramic composite.
2, the high-compactness quartz/quartz composite material provided by the invention based on freeze drying process is compiled with quartz fibre
Fabric is reinforced phase, using silica as matrix；In the composite material volume fraction of silica fibrage object be 40~
47%；The composite material can be applied to antenna house, antenna windows and other aerospace fields.
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 the high-compactness quartz/quartz composite material and preparation method thereof process provided by the invention based on freeze-drying
Figure；
Fig. 2 is high-compactness quartz/quartz composite density Gradient mode figure prepared by embodiment 1.
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-compactness quartz/quartz composite material based on freeze drying process, the composite wood
Material is using silica fibrage object as reinforced phase, using silica as matrix；The body of silica fibrage object in the composite material
Fraction is 40~47%；The composite material can be applied to antenna house, antenna windows and other aerospace fields.
The density of the composite material is 1.65~1.75g/cm3, bending strength is 70.0~80.5MPa.
It is verified through a large number of experiments, it is multiple when the volume fraction of the silica fibrage object that reinforced phase uses is 40%~47%
Condensation material has excellent mechanical strength and heat-resisting quantity, can meet quartz/quartz composite material well in antenna house, day
The application demand of line window and other aerospace fields.Meanwhile the composite material consistency is high, density gradient is small, mechanical property
It is excellent.
The present invention also proposes a kind of high-compactness quartz/quartz composite material and preparation method thereof based on freeze drying process,
As shown in Figure 1, comprising the following steps:
S1: being placed in immersion treatment in organic solvent for silica fibrage object, to remove silica fibrage object surface
The impurity such as dust, size dry spare after the completion of impregnating；
The weaving manner of the silica fibrage object is that 2.5D weaves or 3 D multi-directional weaves.
Silica fibrage object is woven to suitable shape according to actual needs by the silica fibrage object thickness
Shape and size.
Preferably, the organic solvent is at least one of acetone, dehydrated alcohol and dimethylbenzene, selects suitable volume
The impurity such as dust, the organism for removing silica fibrage object surface with faster and better dissolution.
Preferably, the time of the immersion treatment is 4~6h, repeats to impregnate 3 times, to guarantee silica fibrage object surface
The impurity removal such as dust, organism it is clean.
S2: vacuum impregnation will be carried out by the silica fibrage object of step S1, freeze-drying work is carried out after the completion of dipping
Skill repeats the vacuum impregnation and freeze drying process process 3~4 times, makes the silica substrate fiberfill fibers of greater particle size
Braided part overall skeleton；The vacuum-impregnated impregnating agent is the silicon sol solution that solute partial size is 40~50nm；Preferable particle size
For 50nm；
S3: vacuum impregnation and freeze drying process process 2~3 will be continued by the silica fibrage object of step S2
It is secondary, so that the silica substrate of small particle is sufficient filling with material hole, keep material full densificationization compound, until no longer weight gain is
Only；The vacuum-impregnated impregnating agent is the silicon sol solution that solute (silica solution, i.e. silica) partial size is 10~20nm；It is excellent
Selecting partial size is 10nm；
Silicon sol solution is injected into impregnating autoclave by the way of vacuum injection silicon sol solution in S2 and S3.Using freezing
Drying process prepares silica substrate, since solvent is uniformly distributed that (solvent is uniformly distributed, i.e., does not reunite in silicon sol solution
There is serious density gradient in precipitating, the basis material that not will lead to preparation), therefore prepared silica substrate is more equal
It is even, and drying can be completed in freeze-dried technique, and silica fibrage object can be protected to keep original size and structure.
Preferably, in the step S2 and S3, the vacuum-impregnated time is 12~16h, and preferably 16h, temperature is room
Temperature.
Preferably, in the step S2 and S3, the freeze drying process includes two stages, and the respectively first stage is cold
Dry, second stage lyophilization is lyophilized.Freeze-drying is first passed through by water congeals into ice in the silica fibrage object after dipping,
Ice is directly distilled by lyophilization again and switchs to steam and remove moisture to complete drying to silica fibrage object.
Preferably, the solidification point of the freeze-drying is -40~-45 DEG C, and freeze-off time is 2~3h, preferably -45 DEG C jellies
Tie 2h；The vacuum degree of the lyophilization is 1.3~13Pa, and temperature is -40~-45 DEG C, and the time is 30~48h, preferably vacuum
Spend 7Pa, -45 DEG C of temperature, time 40h.
Preferably, in the step S2 and S3,18~30wt% of mass fraction of the silicon sol solution, preferred mass point
Number 22% is penetrated into silica fibrage object using silica solution.
S4: final to obtain by being sintered by the silica fibrage object of step S3 to obtain silica substrate
To quartz/quartz composite material.
Preferably, the sintering processes are to keep the temperature temperature at 800 DEG C later from room temperature to 800 DEG C in 2h
It is sintered 1~1.5h, is taken out after cooling to room temperature with the furnace.It is silica that it is guarantee to generate that sintering temperature, which is set as 800 DEG C,
Under the premise of ceramic matrix, mitigate damage of the high temperature to silica fibrage object reinforcement to greatest extent, so that quartz fibre
Braided fabric reinforcement plays more obvious reinforcing effect.Heating rate using 2h from room temperature to 800 DEG C, material internal and outer
Surface is heated more uniformly, avoid generating thermal stress and the generation that leads to crackle.
Preparation method provided by the invention, in silica fibrage object after pretreatment removal of impurities, to silica fibrage
Object carries out vacuum impregnation for several times and freeze drying process process, is finally sintered, obtains quartz/quartz composite material.
In the preparation method, based in dipping process early period, silica fibrage object impregnation channel size is micron dimension, in order to improve
Efficiency of densification is impregnated, preceding 3~4 dippings select the silicon sol solution of big partial size (40~50nm) solute to impregnate, and subsequent 2~3
It is secondary to be impregnated using the silicon sol solution of ultra-small grain size (10~20nm) solute, it is compound to complete densification.Silica solution maceration extract
Middle solute partial size selection principle be it is descending, successively impregnate, first select big partial size silica solution fiberfill fibers braided part entirety bone
Frame, then material hole is sufficient filling with by the dipping of small-grain-diametersilica silica sol, keep material full densificationization compound.In densification process
The silica fibrage object after dipping is dried using freeze drying process, volume is hardly in the drying process for material
Becoming, original structure capable of being kept well, material is in penetrating porous structure after drying, and silica solution enters material when convenient for impregnating again
Material is internal, packing material hole, can further increase densifying materials degree simultaneously reducing density of material gradient, be made close
Spend uniform high-compactness quartz/quartz composite material.Preparation method simple process provided by the invention, short preparation period, at
This is low, can be used for the preparation of the fiber-reinforcement silicon dioxide ceramic composite of Hou Du≤40mm.
Embodiment 1
The present embodiment provides a kind of high-compactness quartz/quartz composite material based on freeze drying process, the composite wood
Material includes reinforced phase and matrix；The reinforced phase is silica fibrage object, and described matrix is silica；The composite material
The volume fraction of middle silica fibrage object is 47%.The silica fibrage object is with a thickness of 40mm.
The present embodiment also provides a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process
Method, comprising the following steps:
S1: the 2.5D structure silica fibrage object of 40mm thickness being placed in acetone and is impregnated, and each soaking time is 4h, weight
It impregnates 3 times, is dried after the completion of impregnating again；
S2: big partial size silicon sol solution Vaccum Permeating is carried out by being placed in impregnating autoclave by the silica fibrage object of step S1
Stain and freezing dry process 4 times are until without obvious weight gain；
The vacuum-impregnated impregnating agent is the silicon sol solution of silica solution mass fraction 18wt%, partial size 40nm, dipping
Time 16h is carried out at room temperature；
S3: by by step S2 silica fibrage object be placed in impregnating autoclave carry out small-grain-diametersilica silica sol vacuum impregnation and
Freeze drying process process 2 times until without obvious weight gain；
The vacuum-impregnated impregnating agent is the silicon sol solution of silica solution mass fraction 22wt%, partial size 20nm, dipping
Time 16h is carried out at room temperature；
In the step S2 and S3, freeze drying process are as follows: -40 DEG C of temperature, time 2h freeze；Vacuum degree 13Pa, temperature
The lyophilization of -40 DEG C of degree, time 36h；
S4: will be sintered by the silica fibrage object of step S3, set sintering condition 2h from room temperature
To 800 DEG C, heat preservation sintering 1h takes out after cooling to room temperature with the furnace, obtains quartz/quartz composite material.
The density for the composite material that the present embodiment is prepared is 1.69g/cm3, composite material is pressed into thickness average mark three
After layer incision (as shown in Figure 2), each layer even density, density gradient is small；The bending strength of gained composite material is 70.8MPa,
Excellent in mechanical performance.
Embodiment 2
The present embodiment provides a kind of high-compactness quartz/quartz composite material based on freeze drying process, the composite wood
Material includes reinforced phase and matrix；The reinforced phase is silica fibrage object, and described matrix is silica；The composite material
The volume fraction of middle silica fibrage object is 43%.The silica fibrage object is with a thickness of 45mm.
The present embodiment also provides a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process
Method, comprising the following steps:
S1: the 2.5D structure silica fibrage object of 45mm thickness is placed in acetone and dimethylbenzene mixed liquor and is impregnated, every time
Soaking time is 5h, repeats to impregnate 3 times, dry after the completion of impregnating；
S2: big partial size silicon sol solution Vaccum Permeating is carried out by being placed in impregnating autoclave by the silica fibrage object of step S1
Stain and freezing dry process 3 times are until without obvious weight gain；
The vacuum-impregnated impregnating agent is the silicon sol solution of silica solution mass fraction 22wt%, partial size 50nm, dipping
Time 16h is carried out at room temperature；
S3: by by step S2 silica fibrage object be placed in impregnating autoclave carry out small-grain-diametersilica silica sol vacuum impregnation and
Freeze drying process process 3 times until without obvious weight gain；
The vacuum-impregnated impregnating agent is the silicon sol solution of silica solution mass fraction 18wt%, partial size 10nm, dipping
Time 16h is carried out at room temperature；
In the step S2 and S3, freeze drying process are as follows: -45 DEG C of temperature, time 2.5h freeze；Vacuum degree 7Pa, temperature
The lyophilization of -45 DEG C of degree, time 40h；
S4: will be sintered by the silica fibrage object of step S3, set sintering condition 2h from room temperature
To 800 DEG C, heat preservation sintering 1.5h takes out after cooling to room temperature with the furnace, obtains quartz/quartz composite material.
The density for the composite material that the present embodiment is prepared is 1.75g/cm3, composite material is pressed into thickness average mark three
After layer is cut, each layer even density, density gradient is small；The bending strength of gained composite material is 76.2MPa, and mechanical property is excellent
It is different.
Embodiment 3
The present embodiment provides a kind of high-compactness quartz/quartz composite material based on freeze drying process, the composite wood
Material includes reinforced phase and matrix；The reinforced phase is silica fibrage object, and described matrix is silica；The composite material
The volume fraction of middle silica fibrage object is 40%.The silica fibrage object is with a thickness of 50mm.
The present embodiment also provides a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process
Method, comprising the following steps:
S1: the 3 D multi-directional structure silica fibrage object of 50mm thickness is placed in acetone and dehydrated alcohol mixed liquor and is soaked
Bubble, each soaking time are 6h, repeat to impregnate 3 times, dry after the completion of impregnating；
S2: big partial size silicon sol solution Vaccum Permeating is carried out by being placed in impregnating autoclave by the silica fibrage object of step S1
Stain and freezing dry process 4 times are until without obvious weight gain；
The vacuum-impregnated impregnating agent is the silicon sol solution of silica solution mass fraction 30wt%, partial size 40nm, dipping
Time 16h is carried out at room temperature；
S3: by by step S2 silica fibrage object be placed in impregnating autoclave carry out small-grain-diametersilica silica sol vacuum impregnation and
Freeze drying process process 3 times until without obvious weight gain；
The vacuum-impregnated impregnating agent is the silicon sol solution of silica solution mass fraction 22wt%, partial size 10nm, dipping
Time 16h is carried out at room temperature；
In the step S2 and S3, freeze drying process are as follows: -45 DEG C of temperature, time 3h freeze；Vacuum degree 2Pa, temperature
The lyophilization of -45 DEG C of degree, time 48h；
S4: will be sintered by the silica fibrage object of step S3, set sintering condition 2h from room temperature
To 800 DEG C, heat preservation sintering 1.5h takes out after cooling to room temperature with the furnace, obtains quartz/quartz composite material.
The density for the composite material that the present embodiment is prepared is 1.74g/cm3, composite material is pressed into thickness average mark three
After layer is cut, each layer even density, density gradient is small；The bending strength of gained composite material is 80.1MPa, and mechanical property is excellent
It is different.
Comparative example 1
This comparative example provides a kind of quartz/quartz composite material of sol-gel method preparation, and the composite material includes to increase
Strong phase and matrix；The reinforced phase is silica fibrage object, and described matrix is silica；Composite wood described in this comparative example
The volume fraction of silica fibrage object is 47% in material.
The process for preparing sol-gel for the quartz/quartz composite material that this comparative example provides, comprising the following steps:
(1) with embodiment 1；
(2) the pretreated silica fibrage object of step (1) is put into impregnating autoclave, introducing mass fraction be 18wt%,
The silicon sol solution of partial size 40nm carries out vacuum impregnation 16h, gelation 36h, the primary densification of completion at 70 DEG C after the completion of dipping
Change process repeats densification process 7 times until without obvious weight gain；
(3) the silica fibrage object that above-mentioned steps (2) obtain is put into impregnating autoclave, introducing mass fraction be 22wt%,
The silicon sol solution of partial size 20nm carries out vacuum impregnation 16h, gelation 36h, the primary densification of completion at 70 DEG C after the completion of dipping
Change process repeats densification process 5 times until without obvious weight gain；
(4) the silica fibrage object reinforcement of above-mentioned completion densification process is put into high temperature Muffle furnace and carries out ceramic
Processing sets sintering condition 2h from room temperature and is warming up to 800 DEG C, and heat preservation sintering 1h takes out after cooling to room temperature with the furnace, obtains stone
English/quartz composite material.
The density for the composite material that this comparative example is prepared is 1.52g/cm3, bending strength 46.8MPa.
Table 1 is the composite material that Examples 1 to 3 is prepared and the composite property that comparative example 1 is prepared comparison
Table.As seen from the table, the composite material consistency being prepared using preparation method provided by the invention is higher, mechanical property is more excellent
It is different.
The composite property contrast table that 1 comparative example 1 of table and Examples 1 to 3 are prepared
| Sample | Density (g/cm3) | Bending strength (MPa) |
| Embodiment 1 | 1.69 | 70.8 |
| Embodiment 2 | 1.75 | 76.2 |
| Embodiment 3 | 1.74 | 80.1 |
| Comparative example 1 | 1.52 | 46.8 |
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-compactness quartz/quartz composite material based on freeze drying process, which is characterized in that the composite material
Using silica fibrage object as reinforced phase, using silica as matrix；The volume of silica fibrage object in the composite material
Score is 40~47%；The composite material can be applied to antenna house, antenna windows and other aerospace fields.
2. a kind of high-compactness quartz/quartz composite material based on freeze drying process as described in claim 1, feature
It is, the density of the composite material is 1.65~1.75g/cm3, bending strength is 70.0~80.5MPa.
3. a kind of high-compactness quartz/quartz composite material and preparation method thereof based on freeze drying process, which is characterized in that including
Following steps:
S1: silica fibrage object is placed in immersion treatment in organic solvent, is dried；
S2: vacuum impregnation will be carried out by the silica fibrage object of step S1, freeze drying process, weight is carried out after the completion of dipping
Answer the vacuum impregnation and freeze drying process process 3~4 times；The vacuum-impregnated impregnating agent be solute partial size be 40~
The silicon sol solution of 50nm；
S3: vacuum impregnation and freeze drying process process 2~3 times will be continued by the silica fibrage object of step S2；
The vacuum-impregnated impregnating agent is the silicon sol solution that solute partial size is 10~20nm；
S4: it will be sintered by step S3 silica fibrage object to obtain silica substrate, finally obtain stone
English/quartz composite material.
4. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 3
Method, which is characterized in that in the step S1, the organic solvent is at least one of acetone, dehydrated alcohol and dimethylbenzene.
5. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 3
Method, which is characterized in that in the step S1, the time of the immersion treatment is 4~6h, repeats to impregnate 3 times.
6. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 3
Method, which is characterized in that in the step S2 and S3, the vacuum-impregnated time is 12~16h, and temperature is room temperature.
7. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 3
Method, which is characterized in that in the step S2 and S3, the freeze drying process includes two stages, and the respectively first stage is cold
Dry, second stage lyophilization is lyophilized.
8. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 7
Method, which is characterized in that the solidification point of the freeze-drying is -40~-45 DEG C, and freeze-off time is 2~3h；The lyophilization
Vacuum degree be 1.3~13Pa, temperature be -40~-45 DEG C, the time be 30~48h.
9. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 3
Method, which is characterized in that in the step S2 and S3,18~30wt% of mass fraction of the silicon sol solution.
10. a kind of high-compactness quartz/quartz composite material preparation side based on freeze drying process as claimed in claim 3
Method, which is characterized in that in the step S4, the sintering processes are by temperature in 2h from room temperature to 800 DEG C, Zhi Hou
1~1.5h of heat preservation sintering at 800 DEG C.
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