CN116750975A - Quartz fiber composite material and preparation method thereof - Google Patents
Quartz fiber composite material and preparation method thereof Download PDFInfo
- Publication number
- CN116750975A CN116750975A CN202311049396.4A CN202311049396A CN116750975A CN 116750975 A CN116750975 A CN 116750975A CN 202311049396 A CN202311049396 A CN 202311049396A CN 116750975 A CN116750975 A CN 116750975A
- Authority
- CN
- China
- Prior art keywords
- quartz fiber
- woven body
- composite material
- mold
- silica sol
- 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
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 239000000835 fiber Substances 0.000 title claims abstract description 139
- 239000010453 quartz Substances 0.000 title claims abstract description 122
- 238000002360 preparation method Methods 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 100
- 238000001035 drying Methods 0.000 claims abstract description 56
- 238000005245 sintering Methods 0.000 claims abstract description 47
- 239000012528 membrane Substances 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims description 58
- 238000000034 method Methods 0.000 claims description 48
- 238000005470 impregnation Methods 0.000 claims description 40
- 238000004321 preservation Methods 0.000 claims description 25
- 238000000280 densification Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000009987 spinning Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000004513 sizing Methods 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 abstract description 19
- 238000001704 evaporation Methods 0.000 abstract description 18
- 230000008020 evaporation Effects 0.000 abstract description 18
- 238000010030 laminating Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 43
- 239000000047 product Substances 0.000 description 28
- 239000000499 gel Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 230000002378 acidificating effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000003754 machining Methods 0.000 description 9
- 239000003733 fiber-reinforced composite Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 239000004744 fabric Substances 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 235000015110 jellies Nutrition 0.000 description 5
- 239000008274 jelly Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 4
- 238000001879 gelation Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/002—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of fibres, filaments, yarns, felts or woven material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
Abstract
The invention discloses a quartz fiber composite material and a preparation method thereof, comprising the steps of putting a pretreated quartz fiber pre-woven body into a porous mold, carrying out dipping operation in a vacuum state, drying the quartz fiber pre-woven body and the porous mold synchronously after the dipping operation is finished, taking out the pre-woven body after the drying is finished, and carrying out high-temperature treatment to obtain a blank; densifying, sintering and processing the blank to obtain a workpiece; densifying and sintering the workpiece to obtain a quartz fiber composite material; the surface laminating of porous mould is provided with one-way ventilated membrane, and one-way ventilated membrane satisfies the vapor and passes through, the unable characteristic of passing through of silica sol. Therefore, by adopting the porous die to carry out the dipping operation on the pre-woven body, the evaporation area is increased compared with that of the non-perforated die, and the evaporation rate is greatly improved, namely the concentration of the silica sol is further improved in the drying process; effectively improves the working efficiency and shortens the preparation period.
Description
Technical Field
The invention relates to the technical field of preparation of high-temperature-resistant wave-transparent composite materials, in particular to a quartz fiber composite material and a preparation method thereof.
Background
The quartz fiber reinforced composite material is a composite material with good comprehensive properties such as dielectric, thermal, mechanical and the like, and is an ideal wave-transmitting material for reentry type and ultra-high speed aircraft radomes. The main molding processes of the quartz fiber reinforced composite material include dip molding, compression molding, slip casting and the like, wherein the dip molding becomes the most commonly used process at present by virtue of the advantages of simple equipment, convenient operation, good product uniformity and the like. The dipping forming is to take quartz fiber pre-woven body as reinforcing phase, obtain blank through pretreatment, dipping, sintering and other procedures, and obtain final product through densification, dampproof and coating treatment after processing to specific size. However, since the solid content of the raw materials used for impregnation is low, repeated impregnation is required to achieve the product performance required for use, and the impregnation period is generally 8 times or more. The actual impregnation effect is not consistent with the theory any more along with the increase of the impregnation period, because the silica sol firstly infiltrates the surface of the woven body, and then gradually expands inwards in different passages, because the silica sol is easy to be accumulated on the surface layer of the woven body, along with the increase of the impregnation period, the impregnation effect is poor, and the core layer and the surface layer of the product generate a larger density gradient to influence the mechanical property and the electrical property of the product, therefore, the surface of the blank needs to be repeatedly machined in the preparation process, thereby leading to complex preparation flow and long preparation period of the product.
The method is characterized in that the method comprises the steps of concentrating commercial acidic silica sol in a reduced pressure rotary evaporation mode to obtain concentrated silica sol with the concentration of 30% -47%, dividing the concentrated silica sol into high-concentration silica sol and medium-concentration silica sol according to different concentration ranges, and designing different densification periods to adopt a combined impregnation scheme of the silica sol with different concentrations.
For example, chinese patent application number CN202111175316.0, publication date 2022, 1 month and 7 days, the patent discloses a high-density fiber reinforced quartz ceramic composite material and its preparation method, and relates to the technical field of composite materials, the method comprises: immersing the fiber preform in the slurry, and then sequentially carrying out vacuum impregnation, drying, sintering and densification to obtain a composite material matrix; and immersing the composite material matrix in silica sol, and then sequentially carrying out vacuum impregnation, drying, sintering and densification to obtain the high-density fiber reinforced quartz ceramic composite material.
The high-concentration silica sol in the two patents has poor stability, and the consistency of the product quality is difficult to ensure in the actual mass production process.
Disclosure of Invention
The invention aims to solve the problems of long preparation period and poor quality of a quartz fiber reinforced composite material in the prior art. Therefore, the invention provides the quartz fiber composite material and the preparation method thereof, which have the advantages of simple process and short preparation period, can be applied to mass production of the quartz fiber reinforced composite material, and ensure the quality of the quartz fiber reinforced composite material.
In order to solve the problems, the invention provides a preparation method of a quartz fiber composite material, which comprises the following steps:
placing the pretreated quartz fiber pre-woven body into a porous mold, wherein the porous mold is provided with a plurality of through holes, and the through holes are covered with a unidirectional breathable film; the unidirectional breathable film meets the characteristic that water vapor passes through and silica sol cannot pass through;
sealing the opening on the die and the plurality of through holes on the die by adopting a sealing piece; after sealing, vacuumizing the porous mold, and injecting silica sol solution to complete the impregnation operation of the quartz fiber pre-woven body in a vacuum state;
after the impregnation operation is finished, removing a sealing piece on the porous mold, drying the quartz fiber pre-woven body and the porous mold synchronously, and taking the quartz fiber pre-woven body out of the porous mold after the drying is finished, and performing high-temperature treatment to obtain a blank;
densifying, sintering and processing the blank to obtain a workpiece;
and densifying and sintering the workpiece to obtain the quartz fiber composite material.
By adopting the technical scheme, the invention adopts the die with the plurality of through holes in the dipping operation, the surfaces of the dies with the plurality of through holes are attached with the unidirectional breathable films, and in the drying process after the dipping operation is finished, the through holes on the die are only covered by the unidirectional breathable films, at the moment, the air inside and outside the die can freely circulate through the through holes on the die, and the silica sol in the die cannot flow out of the through holes; the arrangement can effectively increase the contact area between the silica sol solution and the air, thereby improving the evaporation area of the silica sol solution, improving the concentration of the silica sol before the silica sol is converted into colloid, realizing the high-concentration silica sol to infiltrate the braiding body through the diffusion effect, effectively improving the working efficiency and shortening the preparation period; then preparing the product meeting the use requirement, wherein the density of the product can reach (1.70+/-0.1) g/cm 3 ；
Since the silica sol solution is SiO 2 Colloidal solutions of particles dispersed in water, which are themselves in a metastable state, have a concentration of silica sol and an ambient temperature that affect the stability of the silica sol, and when the silica sol is devitrified, it changes from a low viscosity liquid to a high viscosity gel. If a traditional non-perforated die is adopted in the blank preparation process, the solution state of the silica sol is converted into gel state after a certain time, and the evaporation rate is limited because the evaporation area is only the opening of the die, so that the concentration of the silica sol can not reach the required concentration; however, if a porous mold is adopted in the blank preparation process and a high-efficiency unidirectional ventilated membrane is matched, the evaporation area is increased by more than 50% compared with that of a non-perforated mold, and the evaporation rate is greatly improved, namely the concentration of the silica sol is further improved in the drying process, so that the blank is achievedPreparing requirements;
sealing elements are arranged at the through holes of the porous mold, so that the impregnation operation of the pretreated quartz fiber pre-woven body in the porous mold in a vacuum state is not affected; the sealing element is detachably arranged on the through hole, so that the sealing element is sealed when the soaking operation is carried out, and is unsealed when the subsequent drying is carried out; the operation is simple and convenient, and the normal orderly operation of each procedure is not influenced;
the whole preparation process is simple in process and short in preparation period, can be applied to batch production of quartz fiber reinforced composite materials, and ensures quality.
Further, the porous mold comprises an outer mold and an inner mold, and a plurality of holes are formed in the outer mold and the inner mold; and the inner surface of the outer mold and the outer surface of the inner mold are respectively provided with a unidirectional ventilated membrane in a fitting way, and the shape of the unidirectional ventilated membrane is respectively matched with the shape of the inner surface of the outer mold and the shape of the outer surface of the inner mold.
By adopting the technical scheme, the workpiece in the porous die is placed between the outer die and the inner die, so that holes are formed in the outer die and the inner die, and the unidirectional breathable films are attached to the inner surface of the outer die and the outer surface of the inner die, so that the whole evaporation area is increased, the concentration of the silica sol before gelatinization is increased, and the efficiency is improved; the shape of the unidirectional ventilated membrane is matched with that of the porous mould, so that the sealing effect of the unidirectional ventilated membrane is ensured, meanwhile, the silica sol is prevented from flowing out of the mould through the holes, and the smooth proceeding of the whole process is ensured.
Further, the densification process of the blank comprises the steps of immersing the blank in a silica sol solution for vacuum impregnation, and drying again after the impregnation operation is completed; wherein the concentration of the silica sol solution in the impregnated quartz fiber preform is higher than the concentration of the silica sol solution in the impregnated blank. The high-concentration silica sol solution is adopted in the process of impregnating the quartz fiber pre-woven body, and the low-concentration silica sol is adopted in the process of impregnating the blank, so that the impregnating effect of the silica sol solution on the woven body can be effectively improved, and the final quartz fiber reinforced composite material is ensured to have better mechanical property and electrical property.
Further, the solid content of silica sol in the impregnated quartz fiber pre-woven body is 38% -42%, the viscosity is less than 10 mpa.s, and the PH is 2-4; the solid content of the silica sol in the impregnated blank is 23% -27%, the viscosity is less than 10 mpa.s, and the PH is 2-4.
Further, the vacuum degree in the dipping operation is less than 96 KPa, and the time of vacuum dipping is 60-120 min.
Further, after the operation of impregnating the quartz fiber pre-woven body is completed, drying the quartz fiber pre-woven body and the porous mold synchronously, wherein the drying temperature is 80-120 ℃; the drying process ends with the transition of the silica sol from a liquid state to a gel state.
Further, after the drying is finished, the quartz fiber pre-woven body is subjected to high-temperature treatment, which specifically comprises the steps of heating the quartz fiber pre-woven body to 400-600 ℃, heating the quartz fiber pre-woven body at a heating rate of 10-20 ℃/min and keeping the temperature for 120-240 min.
Further, the heating temperature of the two times of sintering is 600-800 ℃, the heating rate is 10-20 ℃ per minute, and the heat preservation time is 180-360 minutes.
Further, the pre-treatment of the quartz fiber pre-woven body comprises the steps of removing the impregnating compound from the quartz fiber pre-woven body in the fiber spinning process; and the heating temperature in the pretreatment process is 400-600 ℃, the heating rate is 10-20 ℃ per minute, and the heat preservation time is 120-240 minutes.
Further, the impregnation operation and densification operation are cycled several times according to the product density requirements.
A quartz fiber composite material prepared by the method for preparing the quartz fiber composite material according to any one of the above, wherein the density of the quartz fiber composite material is (1.70+ -0.1) g/cm 3 。
By adopting the technical scheme, the quartz fiber composite material is prepared by the preparation method, and has the advantages of low processing cost, short preparation period, low pore space in the quartz fiber composite material, high density and good quality.
Advantageous effects
According to the invention, the porous die is adopted to carry out dipping operation on the quartz fiber pre-woven body, so that the evaporation area is increased compared with that of the non-perforated die, and the evaporation rate is greatly improved, namely, the concentration of silica sol is further improved in the drying process; meanwhile, the arrangement of the sealing element ensures that the die is provided with a plurality of through holes, so that the pre-treated pre-woven body is not affected to carry out dipping operation in the die in a vacuum state; the sealing element is detachably arranged on the through hole, so that the sealing element is sealed when the soaking operation is carried out, and is unsealed when the subsequent drying is carried out; the operation is simple and convenient, and the normal orderly operation of each procedure is not influenced; effectively improves the working efficiency and shortens the preparation period.
Drawings
FIG. 1 is a schematic illustration of blank preparation;
FIG. 2 is a flow chart of the present invention.
In the figure: 1. an outer mold; 2. an inner mold; 3. a unidirectional breathable film; 4. a through hole; 5. quartz fiber pre-weaving body; 6. a cover body; 7. a vacuum pumping port; 8. a silica sol solution injection port; 9. and (5) sealing the cover.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present specification, by describing the embodiments of the present invention with specific examples. While the description of the invention will be described in connection with the preferred embodiments, it is not intended to limit the inventive features to the implementation. Rather, the purpose of the invention described in connection with the embodiments is to cover other alternatives or modifications, which may be extended by the claims based on the invention. The following description contains many specific details for the purpose of providing a thorough understanding of the present invention. The invention may be practiced without these specific details. Furthermore, some specific details are omitted from the description in order to avoid obscuring the invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
It should be noted that in this specification, like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
As shown in fig. 1 and 2, the invention provides a preparation method of a quartz fiber composite material, which comprises the following steps:
step 1, placing a pretreated quartz fiber pre-woven body 5 into a porous mold, wherein the porous mold is provided with a plurality of through holes 4, and the through holes 4 are covered with a unidirectional breathable film 3; the unidirectional ventilated membrane 3 meets the characteristic that water vapor passes through and silica sol cannot pass through;
sealing the opening on the die and the plurality of through holes 4 on the die by adopting a sealing piece; after sealing, carrying out vacuumizing operation on the porous mould, and then injecting silica sol solution to enable the quartz fiber pre-woven body 5 to finish dipping operation in a vacuum state;
the porous mould in the dipping operation is provided with a plurality of through holes 4, the through holes 4 are covered with a unidirectional ventilated membrane 3, and sealing pieces which are detachably arranged on the through holes 4; the unidirectional ventilated membrane 3 meets the characteristic that water vapor passes through and silica sol cannot pass through;
after the impregnation operation is finished, removing a sealing piece on the porous mold, drying the quartz fiber pre-woven body 5 and the porous mold synchronously, and taking out the quartz fiber pre-woven body 5 from the porous mold after the drying is finished, and performing high-temperature treatment to obtain a blank; the quartz fiber pre-woven body 5 is a quartz fiber woven body, the weaving mode is puncture stitching, and the fiber volume content is 40% -50%;
the sealing elements are arranged at the positions of the plurality of through holes 4 of the porous mold, so that the dipping operation of the pretreated quartz fiber pre-woven body 5 in the porous mold in a vacuum state is not affected; the sealing element is detachably arranged on the through hole 4, so that the sealing element seals when the dipping operation is carried out, and releases the sealing when the subsequent drying is carried out; the operation is simple and convenient, and the normal orderly operation of each procedure is not influenced; the sealing member on the through hole 4 may be a sealing bag, a sealing cover 9, a sealing plug, etc., which is mainly used for sealing the through hole 4, so that the sealing member capable of sealing the through hole 4 on the porous mold can be used in the present invention;
in one embodiment, the sealing element of the porous mold comprises a cover body 6 and a sealing cover 9 for sealing the porous mold, wherein a vacuumizing opening 7 and a silica sol solution injection opening 8 are arranged on the cover body 6, in one use mode, the pretreated quartz fiber pre-woven body 5 is firstly put into the porous mold, then the through holes 4 in the porous mold are sealed by adopting the sealing cover 9, and meanwhile, the openings of the porous mold are sealed by the cover body 6. After the porous mold is completely sealed, the vacuum treatment is carried out in the porous mold through the vacuum-pumping port 7 of the cover body 6, and the vacuum degree is less than 96 Kpa; finally, a high-concentration silica sol solution is injected through the silica sol solution injection port 8. As will be appreciated by those skilled in the art, the pretreated silica fiber pre-woven body 5 has larger pores inside, so that the silica sol solution with high concentration is selected during the impregnation process, so that on one hand, the silica sol solution can be quickly immersed into the pores inside the silica fiber pre-woven body 5, and on the other hand, the water content of the silica sol solution is reduced, so that the subsequent drying rate can be increased, and the silica sol solution can be quickly changed from a liquid state to a gel state.
Carrying out dipping operation on the quartz fiber pre-woven body 5 in a vacuum state, wherein the time of vacuum dipping is 60-120 min;
after the impregnation operation is completed, the cover body 6 and the sealing cover 9 of the porous mold are removed, and then the quartz fiber pre-woven body 5 and the porous mold are moved into a drying oven together for drying, so that the silica sol solution impregnated by the quartz fiber pre-woven body 5 is converted from a liquid state to a gel state after a certain time (for example, 2-5 days).
After the drying is finished, the silica sol solution is basically changed from a liquid state to a gel state, so that the quartz fiber pre-woven body 5 can be taken out of the porous mold, an electric furnace high-temperature treatment is carried out on the quartz fiber pre-woven body 5 to obtain a blank, the blank is heated to 400-600 ℃ at a heating rate of 10-20 ℃/min, and the heat preservation time is 120-240 min;
the porous mold in the embodiment specifically comprises an outer mold 1 and an inner mold 2, wherein a plurality of through holes 4 are formed in the outer mold 1 and the inner mold 2; the arrangement of a plurality of through holes 4 improves the working efficiency; the inner surface of the outer mold 1 and the outer surface of the inner mold 2 are respectively provided with a unidirectional ventilated membrane 3 in a fitting way, and the shape of the unidirectional ventilated membrane 3 is respectively matched with the shape of the inner surface of the outer mold 1 and the shape of the outer surface of the inner mold 2; the shape of the unidirectional ventilated membrane 3 is matched with the porous mould, so that the unidirectional ventilated membrane 3 can be completely attached to the porous mould, the silica sol is prevented from flowing out of the porous mould through the through hole 4, and the smooth proceeding of the whole process is ensured. Preferably, the unidirectional air permeable membrane 3 can be a VAP unidirectional air permeable membrane, which can not only reduce energy consumption but also save cost. Preferably, the porous mold may be made of stainless steel, aluminum or glass fiber reinforced plastic.
In one embodiment, the through holes 4 on the outer die 1 and the inner die 2 in the porous die are arranged as circular holes, which is beneficial to the processing of the through holes 4. In other alternative embodiments, the shape of the through hole 4 may be hexagonal, octagonal, rectangular, or elongated.
In one embodiment, the through holes 4 on the outer die 1 and the inner die 2 in the porous die are uniformly distributed, so that the strength of the outer die 1 and the inner die 2 can be ensured while the holes are opened, and the phenomenon of uneven strength distribution is not caused. In other alternative embodiments, the plurality of through holes 4 may be arranged in a staggered manner or in a grid shape.
It will be appreciated by those skilled in the art that the shape and arrangement of the through holes 4 are not particularly limited, since the through holes 4 function to allow air to freely circulate through the through holes 4, but the silica sol cannot flow out of the through holes 4.
Step 2, densifying the blank: placing the blank into a conventional mold (the conventional mold is not provided with holes, namely a common accommodating mold), sealing an opening of the conventional mold, vacuumizing, then injecting a low-concentration silica sol solution into the conventional mold, impregnating in a vacuum state, taking the blank out of the conventional mold after the impregnation is finished, and placing the blank into a drying box for drying.
During gelation of the silica sol solution and high-temperature treatment of the quartz fiber pre-woven body 5 in an electric furnace, fine air holes are formed in the blank, so that the density of the blank is reduced; therefore, the blank needs to be subjected to vacuum impregnation and drying again by adopting the low-concentration silica sol solution, so that the silica sol can further fill air holes in the blank, and the density of the blank is improved.
Step 3, sintering: placing the densified blank into an electric furnace for sintering; the specific sintering heating temperature is 600-800 ℃, the heating rate is 10-20 ℃ per minute, and the heat preservation time is 180-360 minutes;
step 4, processing: machining the sintered blank on a machine tool according to the size requirement to obtain a workpiece;
step 5, densification: placing the processed workpiece into a conventional mold, sealing the conventional mold, and performing vacuumizing treatment, wherein the vacuum degree is less than 96 Kpa; then injecting the silica sol into a conventional mold, and impregnating in a vacuum state, wherein the vacuum impregnation time is 60-120 min; and after the impregnation is finished, the workpiece is taken out of the conventional die and put into a drying oven for drying.
In addition, the densified blank may cause voids in the internal structure of the workpiece during sintering and during machining on a machine tool, so that the machined workpiece is densified again to improve the quality of the workpiece.
Step 6, sintering: and (3) placing the densified workpiece into an electric furnace for sintering, wherein the specific sintering heating temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the heat preservation time is 180-360 min.
The two densification processes are conventional dies, and a porous die is not selected, so that in the step 1, when the blank is densified after filling is completed, only small air holes exist in the blank, the concentration of the silica sol is not required to be increased by using the porous die, and the conventional die is matched with the silica sol with lower concentration to fill the small air holes in the blank.
According to the invention, the porous mold is adopted in the impregnation operation, the unidirectional ventilated membrane 3 is attached to the surface of the porous mold, so that the evaporation area can be effectively increased, the concentration of the silica sol before the silica sol is colloidized is improved, the high-concentration silica sol is used for impregnating the braid body through the diffusion effect, the working efficiency is effectively improved, and the preparation period is shortened; then preparing the product meeting the use requirement, wherein the density of the quartz fiber composite material product prepared by the preparation method can reach (1.70+/-0.1) g/cm 3 。
As will be appreciated by those skilled in the art, since the silica sol solution is SiO 2 Colloidal solutions in which the particles are dispersed in water are in a metastable state, and the concentration of the silica sol and the ambient temperature affect its stability, and when the silica sol loses its properties, it changes from a low viscosity liquid to a high viscosity colloid. If a traditional non-perforated die is adopted in the blank preparation process, the state of the silica sol solution is changed into gel state after a certain time, and the evaporation rate is limited because the evaporation area is only the opening of the die, so that the concentration of the silica sol solution can not reach the required concentration; however, if a porous die is adopted in the blank preparation process and a high-efficiency unidirectional ventilated membrane 3 is matched, the evaporation area is increased compared with that of a die without holes, and the evaporation rate is greatly improved, namely the concentration of silica sol is further improved in the drying process, so that the blank preparation requirement is met;
the whole preparation process is simple in process and short in preparation period, can be applied to batch production of quartz fiber reinforced composite materials, and ensures quality.
In one embodiment, the sum of the areas of the plurality of through holes 4 in the porous mold may be greater than 10% or more of the area of the mold opening, e.g., 15%, 20%, 30%, 50%, 80%, 110%; thereby increasing the evaporation area by a corresponding ratio to increase the evaporation rate of the silica sol. Specifically, the sum of the areas of the plurality of through holes 4 in the porous mold may be set according to the requirement of the evaporation rate.
In one embodiment, the pore diameter of the plurality of through holes 4 in the porous mold can be 3-5 cm, so that the unidirectional breathable film 3 can better cover the through holes 4. In other embodiments, the pore size of the plurality of through holes 4 in the porous mold may also be less than 3cm or greater than 5cm.
In one embodiment, the preparation method of the quartz fiber composite material comprises blank preparation and twice densification, wherein the concentration of silica sol adopted in the impregnation process in the blank preparation is higher than that in the subsequent densification process; the densification efficiency can be improved by adopting a matching mode of firstly high-concentration silica sol and then low-concentration silica sol, so that the micelle can smoothly permeate inwards, and the high-density performance of the material preparation is ensured. Specifically, in the present example, the silica sol has a solids content of 38% -42% and a viscosity of < 10 mpa.s and a pH of 2-4 in the dipping operation; the solid content of the silica sol in the densification operation is 23% -27%, the viscosity is less than 10 mpa.s, and the PH is 2-4.
And the dipping operation and the densification operation are circulated several times according to the product density requirement. The number of cycles can be selected based on the field conditions and the final product.
In one embodiment, pre-treating the pre-woven body includes removing a sizing agent from the pre-woven body during the fiber spinning process; the heating temperature in the pretreatment process is 400-600 ℃, the heating rate is 10-20 ℃ per minute, and the heat preservation time is 120-240 minutes; the heating temperature, the heating rate and the heat preservation time are correspondingly controlled, so that the energy waste is avoided and the pretreatment effect is ensured.
Example 1:
the preparation method of the quartz fiber composite material comprises the following steps:
s1: preparation of a pre-woven body: the quartz fiber pre-woven body 5 is a conical rotary body with the height of 600mm, the thickness of the fabric is 12.2mm, and the fiber volume content is 42.5%;
s2: pretreatment of the pre-woven body: placing the quartz fiber pre-woven body 5 into an electric furnace for pretreatment, wherein the pretreatment temperature is 500 ℃, the pretreatment system is that the temperature is raised for 300min, and the heat preservation time is 180min;
s3: preparing a blank:
s31: placing the pretreated quartz fiber pre-woven body 5 into a porous mold which is pre-attached with a unidirectional breathable film 3, and sealing the porous mold by adopting a sealing element;
s32: vacuumizing the porous mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 40% into the porous mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s33: removing the sealing piece after the vacuum impregnation is finished, and conveying the quartz fiber pre-woven body 5 and the porous mold into a drying box, wherein the drying temperature is set to be 90 ℃;
s34: taking the quartz fiber pre-woven body 5 out of the porous mold after the silica sol solution is gelled, and cleaning up jelly on the surface of the quartz fiber pre-woven body 5;
s35: placing the quartz fiber pre-woven body 5 into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is increased for 300min, and the heat preservation time is 180min;
s4: the blank is densified, and the specific operation is as follows:
s41: placing the blank into a conventional mold and sealing the conventional mold, wherein the conventional mold is not perforated but still has openings, so that the openings of the conventional mold are sealed;
s42: vacuumizing the conventional mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 25% into the conventional mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s43: after the vacuum impregnation is finished, the opening of the conventional mold is unsealed, the blank is taken out of the conventional mold, the drying temperature is set to 180 ℃, and the drying time is set to 120min;
s44: repeating steps S41 to S43;
s5: sintering: placing the workpiece into an electric furnace for sintering, wherein the sintering temperature is 750 ℃, the sintering system is that the temperature is increased for 400min, and the heat preservation time is 180min;
s6: processing: machining the sintered workpiece to a specified size on a numerical control lathe;
s7: and (3) densifying the workpiece: the densification process is the same as step S4;
s8: sintering: the sintering process is the same as step S5.
The prepared product is subjected to sampling at the mouth to test the strength and density, and meanwhile, the whole product is subjected to density test by using a porous ceramic apparent porosity test method, and the test result is shown in the attached table 1.
Example 2:
the preparation method of the quartz fiber composite material comprises the following steps:
s1: preparation of a pre-woven body: the quartz fiber pre-woven body 5 is a conical rotary body with the height of 600mm, the thickness of the fabric is 11.8mm, and the fiber volume content is 42.9%;
s2: pretreatment of the pre-woven body: placing the quartz fiber pre-woven body 5 into an electric furnace for pretreatment, wherein the pretreatment temperature is 500 ℃, the pretreatment system is that the temperature is raised for 300min, and the heat preservation time is 180min;
s3: preparing a blank:
s31: placing the pretreated quartz fiber pre-woven body 5 into a porous mold which is pre-attached with a unidirectional breathable film 3, and sealing the porous mold by adopting a sealing element;
s32: vacuumizing the porous mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 40% into the porous mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s33: removing the piece after the vacuum impregnation is finished, and conveying the quartz fiber pre-woven body 5 and the porous mold into a drying box, wherein the drying temperature is set to be 90 ℃;
s34: taking the quartz fiber pre-woven body 5 out of the porous mold after the silica sol is gel, and cleaning up jelly on the surface of the quartz fiber pre-woven body 5;
s35: placing the quartz fiber pre-woven body 5 into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is increased for 300min, and the heat preservation time is 180min;
repeating the steps S31 to S35;
s4: the blank is densified, and the densification is consistent with that of the embodiment 1;
s5: sintering: the sintering treatment remained the same as in example 1;
s6: processing: machining the sintered workpiece to a specified size on a numerical control lathe;
s7: the workpiece was densified in accordance with example 1;
s8: sintering: the sintering process was consistent with example 1.
The prepared product is subjected to sampling at the mouth to test the strength and density, and meanwhile, the whole product is subjected to density test by using a porous ceramic apparent porosity test method, and the test result is shown in the attached table 1.
Example 3:
the preparation method of the quartz fiber composite material comprises the following steps:
s1: preparation of a pre-woven body: the quartz fiber pre-woven body 5 is a conical rotary body with the height of 600mm, the thickness of the fabric is 12.5mm, and the fiber volume content is 43.1%;
s2: pretreatment of the pre-woven body: placing the quartz fiber pre-woven body 5 into an electric furnace for pretreatment, wherein the pretreatment temperature is 500 ℃, the pretreatment system is that the temperature is raised for 300min, and the heat preservation time is 180min;
s3: preparing a blank:
s31: placing the pretreated quartz fiber pre-woven body 5 into a porous mold which is pre-attached with a unidirectional breathable film 3, and sealing the porous mold by adopting a sealing element;
s32: vacuumizing the porous mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 40% into the porous mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s33: removing the sealing piece after the vacuum impregnation is finished, and conveying the quartz fiber pre-woven body 5 and the porous mold into a drying box, wherein the drying temperature is set to be 90 ℃;
s34: taking the quartz fiber pre-woven body 5 out of the porous mold after the silica sol is gel, and cleaning up jelly on the surface of the quartz fiber pre-woven body 5;
s35: placing the quartz fiber pre-woven body 5 into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is increased for 300min, and the heat preservation time is 180min;
repeating the steps S31 to S35 for two times to finish the steps S31 to S35 three times;
s4: the blank is densified by one step S44 compared with embodiment 1, that is, the blank is densified by this embodiment only steps S41 to S43 in embodiment 1, that is, the densification is completed;
s5: sintering: the sintering treatment remained the same as in example 1;
s6: processing: machining the sintered workpiece to a specified size on a numerical control lathe;
s7: the workpiece is densified, and compared with the embodiment 1, the densification is performed by one step S44, namely the blank is densified in the embodiment, and the densification is completed only by the steps S41 to S43 in the embodiment 1;
s8: sintering: the sintering process was consistent with example 1.
The prepared product is subjected to sampling at the mouth to test the strength and density, and meanwhile, the whole product is subjected to density test by using a porous ceramic apparent porosity test method, and the test result is shown in the attached table 1.
Example 4:
the preparation method of the quartz fiber composite material comprises the following steps:
s1: preparation of a pre-woven body: the quartz fiber pre-woven body 5 is a cylinder with the height of 300mm, the thickness of the fabric is 12.3mm, and the fiber volume content is 43.2%;
s2: pretreatment of the pre-woven body: placing the quartz fiber pre-woven body 5 into an electric furnace for pretreatment, wherein the pretreatment temperature is 500 ℃, the pretreatment system is that the temperature is raised for 300min, and the heat preservation time is 180min;
s3: preparing a blank:
s31: placing the pretreated quartz fiber pre-woven body 5 into a porous mold which is pre-attached with a unidirectional breathable film 3, and sealing the porous mold by adopting a sealing element;
s32: vacuumizing the porous mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 40% into the porous mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s33: removing the sealing piece after the vacuum impregnation is finished, and conveying the quartz fiber pre-woven body 5 and the porous mold into a drying box, wherein the drying temperature is set to be 90 ℃;
s34: taking the quartz fiber pre-woven body 5 out of the porous mold after the silica sol is gel, and cleaning up jelly on the surface of the quartz fiber pre-woven body 5;
s35: placing the quartz fiber pre-woven body 5 into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is increased for 300min, and the heat preservation time is 180min;
repeating the steps S31 to S35 for 1 time, namely completing the steps S31 to S35 twice;
s4: the blank is densified, and the densification is consistent with that of the embodiment 1;
s5: sintering: the sintering treatment remained the same as in example 1;
s6: processing: machining the sintered workpiece to a specified size on a numerical control lathe;
s7: the workpiece was densified in accordance with example 1;
s8: sintering: the sintering process was consistent with example 1.
The prepared product is subjected to sampling at the mouth to test the strength and density, and meanwhile, the whole product is subjected to density test by using a porous ceramic apparent porosity test method, and the test result is shown in the attached table 1.
Example 5:
the preparation method of the quartz fiber composite material comprises the following steps:
s1: preparation of a pre-woven body: the quartz fiber pre-woven body 5 is a conical rotary body with the height of 300mm, the thickness of the fabric is 30mm, and the fiber volume content is 44.3%;
s2: pretreatment of the pre-woven body: placing the quartz fiber pre-woven body 5 into an electric furnace for pretreatment, wherein the pretreatment temperature is 500 ℃, the pretreatment system is that the temperature is raised for 300min, and the heat preservation time is 180min;
s3: preparing a blank:
s31: placing the pretreated quartz fiber pre-woven body 5 into a porous mold which is pre-attached with a unidirectional breathable film 3, and sealing the porous mold by adopting a sealing element;
s32: vacuumizing the porous mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 40% into the porous mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s33: removing the sealing piece after the vacuum impregnation is finished, and conveying the quartz fiber pre-woven body 5 and the porous mold into a drying box, wherein the drying temperature is set to be 90 ℃;
s34: taking the quartz fiber pre-woven body 5 out of the porous mold after the silica sol is gel, and cleaning up jelly on the surface of the quartz fiber pre-woven body 5;
s35: placing the pre-woven body into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is increased for 300min, and the heat preservation time is 180min;
repeating the steps S31 to S35 for 1 time, namely completing the steps S31 to S35 twice;
s4: the blank is densified, and the densification is consistent with that of the embodiment 1;
s5: sintering: the sintering treatment remained the same as in example 1;
s6: processing: machining the sintered workpiece to a specified size on a numerical control lathe;
s7: the workpiece was densified in accordance with example 1;
s8: sintering: the sintering process was consistent with example 1.
The prepared product is subjected to sampling at the mouth to test the strength and density, and meanwhile, the whole product is subjected to density test by using a porous ceramic apparent porosity test method, and the test result is shown in the attached table 1.
Therefore, the preparation method of the quartz fiber composite material can cope with the preparation of products with various shapes and is also suitable for the preparation of products with various thicknesses; the whole preparation period is short, and the preparation can be completed generally within 12-15 days (wherein the gel process of the silica sol solution is about 3 days, and the sintering and machining processes are about 2-4 days); the bending strength and the overall density are greatly improved compared with the prior art.
After the porous mold is used, in the preparation process of the quartz fiber composite material, when the quartz fiber pre-woven body 5 and the porous mold are dried in a drying box, the time of the gelation process of the silica sol solution is reduced by virtue of the large vaporizable area provided by the porous mold, and the gelation of the silica sol solution can be completed only by 2-3 days.
Comparative example 1
In comparison with example 1, the porous mold and the unidirectional breathable film 3 are not used in the blank preparation process in step S3, and the conventional mold is used for impregnation and gelation treatment, and other steps are the same as in example 1. The final product had an oral density of 1.5 g/cm 3 Compared with the product prepared in example 1, the mouth density of the product is 1.63 g/cm 3 The performance of the product is obviously reduced.
Comparative example 2
A method for preparing a quartz fiber composite material, which comprises the following steps in order to prepare a product with similar density to that of the embodiment 1:
s1: preparation of a pre-woven body: the quartz fiber pre-woven body 5 is a conical rotary body with the height of 600mm, the thickness of the fabric is 12.2mm, and the fiber volume content is 42.8%;
s2: pretreatment of the pre-woven body: placing the quartz fiber pre-woven body 5 into an electric furnace for pretreatment, wherein the pretreatment temperature is 500 ℃, the pretreatment system is that the temperature is raised for 300min, and the heat preservation time is 180min;
s3: preparing a blank:
s31: placing the pretreated quartz fiber pre-woven body 5 into a conventional mold, and sealing the conventional mold;
s32: vacuumizing the conventional mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 40% into the conventional mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s33: removing the sealing device after the vacuum impregnation is finished, taking the quartz fiber pre-woven body 5 out of the conventional die, and putting the quartz fiber pre-woven body into a drying oven, wherein the drying temperature is set to 180 ℃, and the drying time is set to 120min;
s34: repeating steps S31 to S33;
s35: placing the pre-woven body into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is increased for 300min, and the heat preservation time is 180min;
s36: preprocessing: processing the sintered workpiece on a numerical control lathe, and respectively processing 50-100 wires on the inner surface and the outer surface;
s37: repeating steps S31 to S33;
s4: the blank is densified, and the specific operation is as follows:
s41: placing the blank into a mould and sealing a conventional mould;
s42: vacuumizing the conventional mold by using a vacuum pump, injecting an acidic silica sol solution with the solid content of 25% into the conventional mold through a feed inlet when the vacuum degree reaches 100KPa, and immersing for 90min in a vacuum state;
s43: removing the sealing device after the vacuum impregnation is finished, taking the blank out of the conventional die, setting the drying temperature to 180 ℃, and setting the drying time to 120min;
s44: placing the pre-woven body into an electric furnace for high-temperature treatment, wherein the high-temperature treatment temperature is 500 ℃, the high-temperature treatment system is that the temperature is raised by 300 ℃, and the heat preservation time is 180 minutes;
s45: preprocessing: processing the sintered workpiece on a numerical control lathe, and respectively processing 50-100 wires on the inner surface and the outer surface;
s46: repeating steps S41 to S43 for 2 times;
s5: sintering: placing the workpiece into an electric furnace for sintering, wherein the sintering temperature is 750 ℃, the sintering system is that the temperature is increased for 400min, and the heat preservation time is 180min;
s6: processing: machining the sintered workpiece to a specified size on a numerical control lathe;
s7: and (3) densifying the workpiece: the processing method is S41 to S43 in step S4, and loops 2 times;
s8: sintering: the sintering process is the same as step S5.
The final product had an mouth density of 1.64 g/cm 3 However, the pre-processing process is added in the process, and the soaking-drying period of the blank preparation process is one more cycle compared with the embodiment 1, and the soaking-drying period of the blank densification process is one more cycle compared with the embodiment 1. The total preparation cycle was 5 days more than in example 1.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the 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 scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (11)
1. The preparation method of the quartz fiber composite material is characterized by comprising the following steps:
placing the pretreated quartz fiber pre-woven body into a porous mold, wherein the porous mold is provided with a plurality of through holes, and the through holes are covered with a unidirectional breathable film; the unidirectional breathable film meets the characteristic that water vapor passes through and silica sol cannot pass through;
sealing the opening on the die and the plurality of through holes on the die by adopting a sealing piece; after sealing, vacuumizing the porous mold, and injecting silica sol solution to complete the impregnation operation of the quartz fiber pre-woven body in a vacuum state;
after the impregnation operation is finished, removing a sealing piece on the porous mold, drying the quartz fiber pre-woven body and the porous mold synchronously, and taking the quartz fiber pre-woven body out of the porous mold after the drying is finished, and performing high-temperature treatment to obtain a blank;
densifying, sintering and processing the blank to obtain a workpiece;
and densifying and sintering the workpiece to obtain the quartz fiber composite material.
2. The method for preparing a quartz fiber composite material according to claim 1, wherein the porous mold comprises an outer mold and an inner mold, wherein a plurality of holes are formed in the outer mold and the inner mold; and the inner surface of the outer mold and the outer surface of the inner mold are respectively provided with a unidirectional ventilated membrane in a fitting way, and the shape of the unidirectional ventilated membrane is respectively matched with the shape of the inner surface of the outer mold and the shape of the outer surface of the inner mold.
3. The method for preparing a silica fiber composite material according to claim 1, wherein the densification of the blank comprises immersing the blank in a silica sol solution for vacuum impregnation, and drying again after the impregnation operation is completed; wherein the concentration of the silica sol solution in the impregnated quartz fiber preform is higher than the concentration of the silica sol solution in the impregnated blank.
4. A method of preparing a silica fiber composite material according to claim 3, wherein the silica sol impregnated in the silica fiber preform has a solids content of 38% -42%, a viscosity of < 10 mpa-s and a PH of 2-4; the solid content of the silica sol in the impregnated blank is 23% -27%, the viscosity is less than 10 mpa.s, and the PH is 2-4.
5. The method for preparing a silica fiber composite material according to claim 2, wherein the vacuum degree in the impregnation operation is less than 96 KPa, and the time of vacuum impregnation is 60min to 120min.
6. The method for preparing a silica fiber composite material according to claim 5, wherein the silica fiber pre-woven body and the porous mold are dried simultaneously after the operation of impregnating the silica fiber pre-woven body is completed, and the drying temperature is 80 ℃ to 120 ℃; the drying process ends with the transition of the silica sol from a liquid state to a gel state.
7. The method for preparing the quartz fiber composite material according to claim 1, wherein the step of performing high-temperature treatment on the quartz fiber pre-woven body after the drying is finished comprises the step of heating the quartz fiber pre-woven body to 400-600 ℃, wherein the heating rate is 10-20 ℃/min, and the heat preservation time is 120-240 min.
8. The method for preparing the quartz fiber composite material according to claim 1, wherein the heating temperature for the two times of sintering is 600-800 ℃, the heating rate is 10-20 ℃ per minute, and the heat preservation time is 180-360 minutes.
9. The method of preparing a silica fiber composite material according to claim 1, wherein the pre-treating the silica fiber preform comprises removing a sizing agent from the silica fiber preform during fiber spinning; and the heating temperature in the pretreatment process is 400-600 ℃, the heating rate is 10-20 ℃ per minute, and the heat preservation time is 120-240 minutes.
10. The method of preparing a silica fiber composite material according to claim 1 or 9, wherein the steps of impregnating the silica fiber pre-woven body and impregnating the blank are circulated several times according to the product density requirement.
11. A quartz fiber composite, characterized by: a quartz fiber composite material prepared by the method of any of claims 1-10, and having a density of (1.70+ -0.1) g/cm 3 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311049396.4A CN116750975B (en) | 2023-08-21 | 2023-08-21 | Quartz fiber composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311049396.4A CN116750975B (en) | 2023-08-21 | 2023-08-21 | Quartz fiber composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116750975A true CN116750975A (en) | 2023-09-15 |
| CN116750975B CN116750975B (en) | 2023-10-13 |
Family
ID=87951897
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311049396.4A Active CN116750975B (en) | 2023-08-21 | 2023-08-21 | Quartz fiber composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116750975B (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278413A (en) * | 1988-04-28 | 1989-11-08 | Seiko Epson Corp | Production of silica sol |
| 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 |
| CN105130483A (en) * | 2015-06-12 | 2015-12-09 | 湖北三江航天江北机械工程有限公司 | Composite quartz ceramic radome body compression molding method and dedicated compression mold |
| CN107253853A (en) * | 2017-06-16 | 2017-10-17 | 湖北三江航天江北机械工程有限公司 | Surface has the quartzy composite ceramics antenna house preparation method of polytetrafluoroethylene (PTFE) moisture barrier coatings |
| CN110272293A (en) * | 2019-04-11 | 2019-09-24 | 山东工业陶瓷研究设计院有限公司 | A kind of abnormally-structured ceramic matric composite antenna house and preparation method thereof |
| CN110629443A (en) * | 2019-10-21 | 2019-12-31 | 湖北三江航天江北机械工程有限公司 | Shaping method of quartz glass fiber radome fabric |
| CN210752119U (en) * | 2019-08-26 | 2020-06-16 | 湖北金晟远环保科技股份有限公司 | Novel silica sol is concentrated device |
| CN212073259U (en) * | 2020-04-08 | 2020-12-04 | 吴江市南骏纺织有限公司 | VAP unidirectional breathable film |
| CN113501723A (en) * | 2021-08-03 | 2021-10-15 | 宁波曙翔新材料股份有限公司 | Preparation method and device of fiber-reinforced ceramic matrix composite antenna housing/window |
| CN113511879A (en) * | 2021-09-09 | 2021-10-19 | 长沙科航特种织造有限公司 | Quartz fiber reinforced quartz-based composite material and manufacturing method thereof |
-
2023
- 2023-08-21 CN CN202311049396.4A patent/CN116750975B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278413A (en) * | 1988-04-28 | 1989-11-08 | Seiko Epson Corp | Production of silica sol |
| 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 |
| CN105130483A (en) * | 2015-06-12 | 2015-12-09 | 湖北三江航天江北机械工程有限公司 | Composite quartz ceramic radome body compression molding method and dedicated compression mold |
| CN107253853A (en) * | 2017-06-16 | 2017-10-17 | 湖北三江航天江北机械工程有限公司 | Surface has the quartzy composite ceramics antenna house preparation method of polytetrafluoroethylene (PTFE) moisture barrier coatings |
| CN110272293A (en) * | 2019-04-11 | 2019-09-24 | 山东工业陶瓷研究设计院有限公司 | A kind of abnormally-structured ceramic matric composite antenna house and preparation method thereof |
| CN210752119U (en) * | 2019-08-26 | 2020-06-16 | 湖北金晟远环保科技股份有限公司 | Novel silica sol is concentrated device |
| CN110629443A (en) * | 2019-10-21 | 2019-12-31 | 湖北三江航天江北机械工程有限公司 | Shaping method of quartz glass fiber radome fabric |
| CN212073259U (en) * | 2020-04-08 | 2020-12-04 | 吴江市南骏纺织有限公司 | VAP unidirectional breathable film |
| CN113501723A (en) * | 2021-08-03 | 2021-10-15 | 宁波曙翔新材料股份有限公司 | Preparation method and device of fiber-reinforced ceramic matrix composite antenna housing/window |
| CN113511879A (en) * | 2021-09-09 | 2021-10-19 | 长沙科航特种织造有限公司 | Quartz fiber reinforced quartz-based composite material and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116750975B (en) | 2023-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109384459B (en) | Fiber-reinforced silicon dioxide heat-insulating ceramic material and preparation method and application thereof | |
| CN110590339B (en) | Preparation method of alumina ceramic component | |
| CN104609867B (en) | A kind of method for densifying of selective laser sintering ceramic member | |
| CN104393402B (en) | The manufacture method of miniature and thin-walled composite ceramic wave-transparent antenna house | |
| CN109293385B (en) | Fiber-reinforced ceramic matrix composite and preparation method thereof | |
| CN105130483B (en) | Compound quartz pottery antenna covering cover body compression-molding method and its special compression mould | |
| CN109400194B (en) | Fiber-reinforced ceramic matrix composite material antenna housing for W wave band and preparation method thereof | |
| CN107602127B (en) | SiC hollow sphere and preparation method thereof | |
| CN103601479A (en) | Preparation method for high-temperature-resistant ultra-thin antenna window | |
| CN110642634A (en) | C/SiC-ZrB2Composite material and preparation method thereof | |
| CN114409420A (en) | Alumina fiber reinforced mullite ceramic matrix composite and preparation method thereof | |
| CN113788695A (en) | Method for forming fiber-reinforced silicon dioxide ceramic composite material | |
| CN111285694A (en) | Preparation method of high-temperature wave-transparent silicon nitride radome | |
| CN115636681B (en) | Nitride fiber reinforced silicon nitride composite material and preparation method and application thereof | |
| CN113800922A (en) | Silica sol dipping composite forming method for quartz fiber braided body | |
| CN116750975B (en) | Quartz fiber composite material and preparation method thereof | |
| CN114455961A (en) | Preparation method of alumina fiber reinforced ceramic composite material containing mullite interface layer | |
| CN113511879A (en) | Quartz fiber reinforced quartz-based composite material and manufacturing method thereof | |
| CN114671697A (en) | Preparation method of SiC/SiC composite material complex rib structure skin | |
| CN111302820A (en) | Preparation method of C/SiC composite material | |
| CN109180194B (en) | Composite densification method for impregnation cracking of precursors in different states of SiC-based composite material | |
| CN105948810B (en) | A kind of three-dimensional netted through-hole composite material and its preparation | |
| CN109016722B (en) | Anti-scouring aerogel composite material and preparation method thereof | |
| CN114455962A (en) | Preparation method of alumina fiber reinforced ceramic matrix composite | |
| CN109503114B (en) | Preparation method of wave-transparent ablation heat-insulation integrated 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 |