CN115636683A - Fiber mixed fabric reinforced quartz-based composite material and preparation method thereof - Google Patents
Fiber mixed fabric reinforced quartz-based composite material and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 267
- 239000004744 fabric Substances 0.000 title claims abstract description 246
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 174
- 239000010453 quartz Substances 0.000 title claims abstract description 169
- 239000002131 composite material Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 94
- 239000004917 carbon fiber Substances 0.000 claims abstract description 94
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000010410 layer Substances 0.000 claims abstract description 53
- 239000012792 core layer Substances 0.000 claims abstract description 25
- 239000002759 woven fabric Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000009941 weaving Methods 0.000 claims description 33
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 29
- 238000009958 sewing Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 23
- 239000012779 reinforcing material Substances 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000003014 reinforcing effect Effects 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 4
- 238000009940 knitting Methods 0.000 description 40
- 230000000052 comparative effect Effects 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 238000002679 ablation Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004080 punching Methods 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention provides a fiber mixed fabric reinforced quartz-based composite material and a preparation method thereof, wherein the reinforced material comprises a first outer layer fiber fabric, a core layer fiber fabric and a second outer layer fiber fabric which are sequentially stacked and connected; the first outer layer fiber fabric and the second outer layer fiber fabric are quartz fiber fabrics; the core layer fiber fabric is a mixed-woven fiber fabric of carbon fibers and quartz fibers or a mixed-woven fiber fabric of quartz fiber cloth and carbon fiber cloth. The fiber mixed woven fabric reinforced quartz-based composite material has the excellent performances of both quartz fiber and carbon fiber, avoids the rapid performance reduction caused by the high-temperature oxidation of the carbon fiber, simultaneously compensates the loss of the high-temperature use performance of the quartz fiber, and has excellent comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic materials, and particularly relates to a fiber mixed woven fabric reinforced quartz-based composite material and a preparation method thereof.
Background
The high-speed aircraft usually uses heat-proof and heat-insulating materials, and along with the continuous development of science and technology, the demands for the heat-proof and heat-insulating materials with low cost, high performance and easy preparation are increasing.
SiO 2f /SiO 2 The composite material has the advantages of light weight, ablation resistance, good heat insulation performance, low radiation coefficient, short preparation period in the process and low cost, and is an ideal material which can be used as an anti-heat insulation material in the fields of aerospace and the like. The quartz fiber is a glassy material and is in a thermodynamically unstable state, a cristobalite phase is easily precipitated at high temperature, and the precipitated cristobalite has a large volume effect in the temperature fluctuation process, so that the fiber is embrittled, the mechanical property of the composite material is greatly reduced, and the use of the composite material at high temperature is severely restricted.
C f /SiO 2 The composite material combines the excellent high-temperature performance of the carbon fiber and has SiO 2 The matrix has the advantages of good oxidation resistance, wide raw material source and low thermal conductivity, and is a good high-temperature material. Wherein, the carbon fiber has excellent ablation resistance, good mechanical property at high temperature, high service temperature and mature performanceThe carbon fiber reinforced silica is stable, low in price and high in weavability, and is expected to obtain a composite material with good mechanical property. However, carbon fibers are not resistant to oxidation, and carbon materials are oxidized at a temperature of more than 400 ℃ to cause structural damage, material defects and rapid performance reduction, so that oxidation resistance protection is required when the carbon fibers are used in a high-temperature aerobic environment, and the preparation cost is high.
Therefore, it is desirable to provide a composite material which has excellent high-temperature properties, can prevent rapid degradation of properties due to oxidation reaction at high temperatures, and can be widely used for heat insulation members of high-speed aircrafts.
Disclosure of Invention
The invention aims to solve the problem of SiO 2f /SiO 2 The volume effect exists in the temperature fluctuation process of quartz fiber in the composite material, so that the mechanical property of the composite material is reduced, and C f /SiO 2 The composite material has excellent high-temperature performance, but the carbon fiber in the composite material is easy to oxidize at high temperature, so that the performance of the composite material is reduced, and the composite material has the advantages of excellent performance of both the quartz fiber and the carbon fiber, capability of avoiding rapid performance reduction caused by high-temperature oxidation of the carbon fiber, capability of making up for loss of high-temperature use performance of the quartz fiber and excellent comprehensive performance.
In order to solve the above problems, the present invention provides in a first aspect a fiber-mixed fabric reinforced quartz-based composite material, comprising a reinforcing material and a quartz matrix;
the reinforced material comprises a first outer layer fiber fabric, a core layer fiber fabric and a second outer layer fiber fabric which are sequentially stacked and connected; the first outer layer fiber fabric and the second outer layer fiber fabric are quartz fiber fabrics; the core layer fiber fabric is a carbon fiber and quartz fiber mixed woven fiber fabric or a quartz fiber cloth and carbon fiber cloth mixed woven fiber fabric.
Preferably, in the reinforcing material, the mass ratio of the quartz fiber to the carbon fiber is (95% -50%): (5% -50%).
Preferably, the mass ratio of the carbon fibers to the quartz fibers in the core layer fiber fabric is (100-30%): (0% -70%).
Preferably, the thickness of the first outer layer fiber fabric is 1-20mm; the thickness of the second outer layer fiber fabric is 1-20mm; the thickness of the core layer fiber fabric is more than or equal to 2mm.
Preferably, in the fiber mixed fabric reinforced quartz-based composite material, the mass content of the reinforced material is 29-50%.
The second aspect of the invention provides a preparation method of the fiber mixed fabric reinforced quartz-based composite material, which comprises the following steps:
s1, performing mixed weaving by adopting quartz fibers and carbon fibers, wherein the weaving method is at least one of three-dimensional orthogonal weaving and 2.5D weaving, or performing needling sewing on quartz fiber cloth and carbon fiber cloth to prepare a mixed weaving fiber fabric prefabricated body;
s2, immersing the hybrid fiber fabric preform by using a solvent, and then drying;
s3, dipping the prefabricated body of the mixed woven fiber fabric processed in the step S2 into silica sol;
s4, curing the hybrid fiber fabric prefabricated body soaked with the silica sol to obtain a hybrid fiber reinforced quartz-based composite material intermediate;
and S5, sintering the intermediate of the hybrid fiber reinforced quartz-based composite material to obtain the fiber hybrid fabric reinforced quartz-based composite material.
Preferably, step S2 specifically includes: placing the mixed woven fiber fabric prefabricated body into a closed container, vacuumizing the closed container, and then sucking the solvent into the closed container under the vacuum condition to immerse the mixed woven fiber fabric prefabricated body; the solvent is at least one of ethanol and acetone; the immersion treatment conditions were: the pressure is 0-10MPa, the temperature is 60-150 ℃, and the treatment time is 2-24 hours.
Preferably, in the step S2, the drying temperature is 60-200 ℃, and the drying time is 10-30 hours.
Preferably, step S3 specifically includes: placing the prefabricated body of the mixed woven fiber fabric processed in the step S2 into a closed container, vacuumizing the closed container, and then carrying out vacuum treatment on the closed containerThen, enabling the closed container to suck silica sol under the vacuum condition, and enabling the hybrid fiber fabric preform to be soaked in the silica sol; siO in silica sol 2 The mass concentration of the silica sol is 20 to 80 percent, and the density of the silica sol is 1.00 to 1.65g/cm 3 。
Preferably, in the step S4, the curing temperature is 100-250 ℃, and the curing time is 24-120h;
in the step S5, the sintering atmosphere is at least one of nitrogen, ammonia and argon or a vacuum environment, the sintering temperature is 300-1000 ℃, and the sintering time is 1-5h.
Preferably, after step S5, the method further comprises: s6, repeating the step S3, the step S4 and the step S5 to 10 times to densify the fiber hybrid fabric reinforced quartz-based composite material.
Compared with the prior art, the invention has the following beneficial effects:
according to the fiber mixed fabric reinforced quartz-based composite material, the mixed fabric of quartz fibers and carbon fibers or the mixed fabric of quartz fiber cloth and carbon fiber cloth is used as a reinforcing material of the composite material, the carbon fibers and the quartz fibers in the material are mixed and reinforced, so that the excellent high-temperature performance of the carbon fibers can be embodied at high temperature, the oxidation reaction of the carbon fibers at high temperature can be prevented, the composite material has excellent comprehensive performance, and the application prospect in the field of high-speed aircraft heat-insulation components is wide.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below with reference to embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
SiO 2f /SiO 2 The composite material used as an anti-heat insulation material has the advantages of light weight, ablation resistance, good heat insulation performance, low radiation coefficient, short preparation period, low cost and the like, wherein the quartz fiber has higher electrical insulation propertyThe performance, dielectric property, corrosion resistance, thermal shock resistance, chemical property and stability are excellent, but the quartz fiber is easy to precipitate a cristobalite phase at high temperature, so that the mechanical property of the composite material is greatly reduced. C f /SiO 2 The composite material combines the excellent high-temperature performance of the carbon fiber and has SiO 2 The carbon fiber has excellent ablation resistance, good mechanical property at high temperature, high use temperature, mature and stable performance, low price and strong weavability of weaving, but the carbon fiber is not anti-oxidation and can be oxidized at the temperature of more than 400 ℃, so that the performance of the composite material is rapidly reduced.
To this end, in a first aspect, an embodiment of the present invention provides a fiber-mixed fabric reinforced quartz-based composite material, including a reinforcing material and a quartz matrix:
the reinforced material comprises a first outer layer fiber fabric, a core layer fiber fabric and a second outer layer fiber fabric which are sequentially stacked and connected; the first outer layer fiber fabric and the second outer layer fiber fabric are quartz fiber fabrics; the core layer fiber fabric is a carbon fiber and quartz fiber mixed woven fabric or a quartz fiber cloth and carbon fiber cloth mixed woven fabric.
According to the fiber mixed woven fabric reinforced quartz-based composite material disclosed by the embodiment of the invention, the quartz-based composite material reinforced by the quartz fiber fabric at the outer layer is adopted, the quartz-based composite material reinforced by the quartz fiber and carbon fiber mixed woven fabric at the inner layer is adopted, and the carbon fiber and the quartz fiber mixed woven fabric in the material are reinforced to be molten at high temperature, so that a protective layer is formed on the surface layer of the composite material, oxygen can be prevented from entering the composite material, and the effect of preventing the carbon fiber from being oxidized at high temperature is achieved.
The above-mentioned connection of the first outer layer fibre fabric, the core layer fibre fabric and the second outer layer fibre fabric is formed in a weaving process, i.e. a weaving connection.
Preferably, in the reinforcing material, the mass ratio of the quartz fiber to the carbon fiber is (95% -50%): (5% -50%).
In the fiber mixed fabric reinforced quartz-based composite material provided by the embodiment of the invention, the ratio of quartz fibers to carbon fibers is not selected at will, the ratio of quartz fibers is too high, the quartz fibers are subjected to crystal transformation and crystallization when used at high temperature, so that the failure strength of the fibers is reduced, the ratio of carbon fibers is too high, a carbon fiber reinforced area is close to the outer side of the composite material, and the carbon fibers are easily oxidized closer to the outer layer under the high temperature condition, so that the carbon fibers are oxidized, and the strength of the composite material is reduced. Experimental research shows that when the proportion is adopted for mixed weaving, the outer quartz fiber fabric layer can be ensured to be molten at high temperature, a protective layer is formed on the surface layer of the composite material, oxygen is prevented from entering the composite material, the effect of preventing carbon fibers from being oxidized is achieved, the core layer mixed weaving fabric can keep high mechanical property in a high-temperature oxygen-free environment, and the effect of improving the high-temperature mechanical property of the composite material is obvious.
The core layer fiber fabric can be a carbon fiber and quartz fiber mixed fabric, a quartz fiber cloth and carbon fiber cloth mixed fabric, a carbon fiber, carbon fiber cloth and quartz fiber cloth mixed fabric, a quartz fiber, carbon fiber mixed fabric, carbon fiber cloth and quartz fiber cloth mixed fabric, and fiber cloth connected through needling sewing. Preferably, the core layer fiber fabric is a mixed woven fabric obtained by needling and sewing carbon fiber cloth and quartz fiber cloth, and specifically is a mixed woven fabric obtained by needling and sewing different carbon fiber cloth layers and quartz fiber cloth layers.
In some embodiments, the distribution of the carbon fibers and the quartz fibers of the hybrid fiber fabric of the core layer fiber fabric may be adjusted according to actual needs, for example, the carbon fibers and the quartz fibers may be uniformly distributed in the hybrid fiber fabric, that is, the ratio of the carbon fibers to the quartz fibers in each layer of the woven structure is the same, or may be set as that in the hybrid fiber fabric, the outer layer is made of pure quartz fibers, the core layer is made of the carbon fibers and the quartz fibers, and the ratio of the carbon fibers is gradually increased and the ratio of the quartz fibers is gradually decreased from the outer layer to the inner layer of the fabric.
In some embodiments, the mass ratio of the carbon fiber to the quartz fiber in the core layer fiber fabric is wide in a selectable range, and preferably, the mass ratio of the carbon fiber to the quartz fiber in the core layer fiber fabric is (100% -30%): (0% -70%). By adopting the proportion, the raw material cost caused by the fact that carbon fibers are completely used can be reduced, the requirement of the composite material on high-temperature mechanical property is met, the risk of reliability reduction caused by high-temperature failure of the quartz fibers of the core layer is reduced, and the high-temperature mechanical property of the composite material is effectively guaranteed.
In some embodiments, the thickness of the outer layer fiber fabric and the thickness of the core layer fiber fabric can be selected in a wide range, and preferably, the thickness of the first outer layer fiber fabric is 1-20mm; the thickness of the second outer layer fiber fabric is 1-20mm; the thickness of the core layer fiber fabric is more than or equal to 2mm. The thickness of the outer quartz fiber fabric layer is small, molten quartz is insufficient to cover the surface of the composite material in a high-temperature environment, and oxygen cannot be effectively prevented from entering the composite material; the thickness of the quartz fiber fabric layer is large, the proportion of the quartz fiber reinforced quartz composite material in a product is large, the loss of mechanical properties at high temperature is large, the reliability is reduced, the thickness of the core layer fabric is small, the effect of effectively supporting the high-temperature mechanical properties of the composite material cannot be achieved by reducing the proportion of carbon fibers in the composite material, when the thickness is adopted, the quartz fibers and the comprehensive proportion of carbon fibers can be comprehensively coordinated, the sufficient ablation amount of the outer quartz fiber fabric layer is ensured, the effects of preventing oxygen from entering the interior of the composite material and insulating heat can be achieved, and meanwhile, the sufficient bearing mechanical effect can be achieved by the inner core layer mixed woven fabric layer.
In some embodiments, the fiber-mixed fabric reinforced quartz-based composite material has a wide mass content range, and can adopt the conventional reinforcing material proportion. Preferably, in the fiber hybrid fabric reinforced quartz-based composite material, the mass content of the reinforcing material is (29% -50%).
The second aspect of the embodiment of the present invention provides a preparation method of the above fiber hybrid fabric reinforced quartz-based composite material, including the following steps:
s1, performing mixed weaving by adopting quartz fibers and carbon fibers, wherein the weaving method is at least one of three-dimensional orthogonal weaving and 2.5D weaving, or performing needling sewing on quartz fiber cloth and carbon fiber cloth to prepare a mixed weaving fiber fabric prefabricated body;
s2, immersing the hybrid fiber fabric preform by using a solvent, and then drying;
s3, dipping the prefabricated body of the mixed woven fiber fabric processed in the step S2 into silica sol;
s4, curing the hybrid fiber fabric prefabricated body soaked with the silica sol to obtain a hybrid fiber reinforced quartz-based composite material intermediate;
and S5, sintering the intermediate of the hybrid fiber reinforced quartz-based composite material to obtain the fiber hybrid fabric reinforced quartz-based composite material.
According to the preparation method of the fiber mixed woven fabric reinforced quartz-based composite material, the carbon fibers and the quartz fibers are mixed and woven to obtain the mixed woven fabric, then the sol-gel process is adopted to prepare the inorganic fiber mixed woven fabric reinforced quartz-based composite material, the carbon fibers and the quartz fibers in the material are mixed and reinforced, the carbon fibers can show excellent high-temperature performance in the use process at high temperature, the oxidation reaction of the carbon fibers at high temperature can be prevented, the comprehensive performance is excellent, and the application prospect in the field of high-speed aircraft heat-insulation-prevention parts is wide.
Preferably, step S2 specifically includes: and placing the mixed woven fiber fabric prefabricated body into a closed container, vacuumizing the closed container, and then sucking the solvent into the closed container under the vacuum condition to immerse the mixed woven fiber fabric prefabricated body.
In some embodiments, the step S2 is to clean the fibers in the hybrid fiber fabric preform, wherein the solvent is selected from a wide range as long as the dirt remained on the fibers can be washed away, and preferably, the solvent is at least one of ethanol and acetone.
In some embodiments, the treatment conditions for the immersion in step S2 are not particularly limited. Preferably, the immersion treatment conditions are: the pressure is 0-10MPa, the temperature is 60-150 ℃, and the treatment time is 2-24 hours.
In some embodiments, the drying temperature and time in step S2 are not particularly limited. Preferably, in the step S2, the drying temperature is 60-200 ℃, and the drying time is 10-30 hours.
In some embodiments, preferably, step S3 specifically includes: and (3) placing the mixed woven fiber fabric prefabricated body processed in the step (S2) in a closed container, vacuumizing the closed container, and then sucking silica sol into the closed container under a vacuum condition to immerse the mixed woven fiber fabric prefabricated body in the silica sol.
In some embodiments, siO in silica sol 2 Has wide selection range of mass concentration and density of the silica sol, preferably SiO in the silica sol 2 The mass concentration of the silica sol is 20 to 80 percent, and the density of the silica sol is 1.00 to 1.65g/cm 3 The silica sol can be better ensured to fully enter the pores of the fiber fabric and submerge the fabric.
In some embodiments, the curing conditions are not particularly limited. Preferably, in step S4, the curing temperature is 100-250 ℃, and the curing time is 24-120h.
In some embodiments, the sintering conditions are not particularly limited. Preferably, in step S5, the sintering atmosphere is at least one of nitrogen, ammonia, and argon, or a vacuum environment, the sintering temperature is 300-1000 ℃, and the sintering time is 1-5h.
In some embodiments, preferably, after step S5, further comprising: s6, repeating the step S3, the step S4 and the step S5 to 10 times to densify the fiber hybrid fabric reinforced quartz-based composite material. Thus, the hybrid fiber reinforced quartz-based composite material with higher densification degree can be obtained.
Examples
Example 1
The preparation method of the fiber mixed fabric reinforced quartz-based composite material comprises the following steps:
s1, performing mixed weaving by using quartz fiber cloth and carbon fiber cloth, wherein the weaving method is needle-punching sewing weaving and preparing a mixed weaving fiber fabric prefabricated body, and specifically comprises the steps of performing needle-punching sewing weaving by using the quartz fiber cloth until the thickness of the quartz fiber fabric is 2mm, then performing needle-punching sewing weaving by using the carbon fiber cloth and the quartz fiber cloth until the thickness of the mixed weaving fiber fabric is 3mm, wherein in the mixed weaving fiber fabric, the mass ratio of the carbon fiber to the quartz fiber is 9:1, then continuing performing needle-punching sewing weaving by using the quartz fiber cloth until the thickness of the quartz fiber fabric is 2mm, and finally obtaining the mixed weaving fiber fabric prefabricated body, wherein the mass ratio of the quartz fiber to the carbon fiber is 65;
s2, placing the mixed woven fiber fabric prefabricated body into a closed container, vacuumizing the closed container, then enabling the closed container to suck ethanol under a vacuum condition, and immersing the mixed woven fiber fabric prefabricated body, wherein the immersing treatment condition is as follows: the pressure is 5MPa, the temperature is 100 ℃, the processing time is 16 hours, and then the drying is carried out, the drying temperature is 120 ℃, and the drying time is 20 hours;
s3, placing the mixed woven fiber fabric prefabricated body processed in the step S2 into a closed container, vacuumizing the closed container, and then enabling the closed container to suck silica sol under a vacuum condition to enable the mixed woven fiber fabric prefabricated body to be soaked in the silica sol; siO in silica sol 2 Has a mass concentration of 30% and a silica sol density of 1.20g/cm 3 ；
S4, curing the hybrid fiber fabric prefabricated body soaked with the silica sol to obtain a hybrid fiber reinforced quartz-based composite material intermediate, wherein the curing temperature is 250 ℃, and the curing time is 26 hours;
s5, sintering the hybrid fiber reinforced quartz-based composite material intermediate in a nitrogen atmosphere at 900 ℃ for 1h.
S6, repeating the step S3, the step S4 and the step S5 times to densify the fiber mixed fabric reinforced quartz-based composite material, and obtaining the fiber mixed fabric reinforced quartz-based composite material.
Example 2
The remaining steps of the preparation method of the fiber-mixed fabric reinforced quartz-based composite material of the embodiment are the same as those of embodiment 1, except that the thicknesses of the first outer layer fiber fabric, the second outer layer fiber fabric and the inner layer mixed fabric are different from those of embodiment 1, and step S1 is as follows:
s1, performing mixed knitting by adopting quartz fiber cloth and carbon fiber cloth, wherein the knitting method is needle sewing knitting to prepare a mixed knitting fiber fabric preform, and specifically, the quartz fiber cloth is adopted to perform needle sewing knitting to obtain a quartz fiber fabric with the thickness of 5mm, then the carbon fiber cloth and the quartz fiber cloth are adopted to perform needle sewing knitting to obtain a mixed knitting fiber fabric with the thickness of 6mm, the mass ratio of the carbon fiber to the quartz fiber in the mixed knitting fiber fabric is 8:2, the quartz fiber cloth is continuously used to perform needle sewing knitting to obtain a quartz fiber fabric with the thickness of 5mm, and the mass ratio of the quartz fiber to the carbon fiber in the finally obtained mixed knitting fiber fabric preform is 73.
Example 3
The remaining steps of the preparation method of the fiber-mixed fabric reinforced quartz-based composite material of the embodiment are the same as those of embodiment 1, except that the thicknesses of the first outer layer fiber fabric, the second outer layer fiber fabric and the inner layer mixed fabric are different from those of embodiment 1, and step S1 is as follows:
s1, performing mixed knitting by adopting quartz fiber cloth and carbon fiber cloth, wherein the knitting method is needle sewing knitting to prepare a mixed knitting fiber fabric preform, and specifically, the quartz fiber cloth is adopted to perform needle sewing knitting to obtain a quartz fiber fabric with the thickness of 8mm, then the carbon fiber cloth and the quartz fiber cloth are adopted to perform needle sewing knitting to obtain a mixed knitting fiber fabric with the thickness of 25mm, the mass ratio of the carbon fiber to the quartz fiber in the mixed knitting fiber fabric is 7:3, the quartz fiber cloth is continuously used to perform needle sewing knitting to obtain a quartz fiber fabric with the thickness of 6mm, and the mass ratio of the quartz fiber to the carbon fiber in the finally obtained mixed knitting fiber fabric preform is 51.
Example 4
The remaining steps of the preparation method of the fiber-mixed fabric reinforced quartz-based composite material of the embodiment are the same as those of embodiment 1, except that the thicknesses of the first outer layer fiber fabric, the second outer layer fiber fabric and the inner layer mixed fabric are different from those of embodiment 1, and step S1 is as follows:
s1, performing mixed knitting by adopting quartz fiber cloth and carbon fiber cloth, wherein the knitting method is needle sewing knitting to prepare a mixed knitting fiber fabric preform, and specifically, the quartz fiber cloth is adopted to perform needle sewing knitting to a quartz fiber fabric with the thickness of 22mm, then the carbon fiber cloth and the quartz fiber cloth are adopted to perform needle sewing knitting to a mixed knitting fiber fabric with the thickness of 1mm, in the mixed knitting fiber fabric, the mass ratio of the carbon fiber to the quartz fiber is 1:9, then the quartz fiber cloth is continuously used to perform needle sewing knitting to a quartz fiber fabric with the thickness of 22mm, and the mass ratio of the quartz fiber to the carbon fiber in the finally obtained mixed knitting fiber fabric preform is 99.8.
Example 5
The remaining steps of the preparation method of the fiber-mixed fabric reinforced quartz-based composite material of the embodiment are the same as those of embodiment 1, except that the thicknesses of the first outer layer fiber fabric, the second outer layer fiber fabric and the inner layer mixed fabric are different from those of embodiment 1, and step S1 is as follows:
s1, performing mixed knitting by adopting quartz fiber cloth and carbon fiber cloth, wherein the knitting method is needle sewing knitting to prepare a mixed knitting fiber fabric preform, specifically, the quartz fiber cloth is adopted to perform needle sewing knitting to obtain a quartz fiber fabric with the thickness of 0.6mm, then the carbon fiber cloth and the quartz fiber cloth are adopted to perform needle sewing knitting to obtain a mixed knitting fiber fabric with the thickness of 1.8mm, in the mixed knitting fiber fabric, the mass ratio of carbon fibers to quartz fibers is 2:8, then the quartz fiber cloth is continuously used to perform needle sewing knitting to obtain a quartz fiber fabric with the thickness of 30mm, and the mass ratio of the quartz fibers to the carbon fibers in the finally obtained mixed knitting fiber fabric preform is 97.6:2.4.
example 6
The remaining steps of the method for preparing a fiber-mixed fabric-reinforced quartz-based composite material of this example are the same as those of example 1, except that the densification process of step S6 is not performed.
Comparative example 1
In the comparative example, a pure quartz fiber fabric is used as a reinforcing material, the weaving method is the same as that in example 1, the thickness of the quartz fiber fabric is the same as that of the prefabricated body of the hybrid fiber fabric in example 1, and the preparation method of the composite material and the mass content of the reinforcing material are the same as those in example 1.
Comparative example 2
In the comparative example, the pure carbon fiber fabric is adopted as the reinforcing material, the weaving method is the same as that in example 1, the thickness of the carbon fiber fabric is the same as that of the prefabricated body of the mixed-woven fiber fabric in example 1, and the preparation method of the composite material and the mass content of the reinforcing material are the same as those in example 1.
Comparative example 3
The remaining steps of the preparation method of the fiber mixed woven fabric reinforced quartz-based composite material of the embodiment are the same as those of the embodiment 1, except that the outer layer does not adopt a pure quartz fiber cloth, but the whole body is woven by adopting the mixed fiber of the carbon fiber cloth and the quartz fiber cloth, and the step S1 is as follows:
s1, adopting carbon fiber cloth and quartz fiber cloth to carry out needling, sewing and weaving until the thickness is 20mm, wherein the mass ratio of the carbon fiber to the quartz fiber in the mixed woven fiber fabric is 8:2.
Performance testing of fiber-reinforced Quartz-based composite materials
The density, tensile strength, and flexural strength of the fiber-reinforced quartz-based composite materials obtained in the examples and comparative examples were measured, and the measurement results are shown in table 1 below. As can be seen from the data in table 1, compared with the composite material using the quartz fiber fabric as the reinforcing material in comparative example 1, the fiber hybrid fabric reinforced quartz-based composite material of the present invention has better strength performance and high temperature performance, compared with the composite material using the carbon fiber fabric as the reinforcing material in comparative example 2, the fiber hybrid fabric reinforced quartz-based composite material of the present invention has better high temperature performance, compared with comparative example 3, which does not have inner and outer layers, and the fiber hybrid fabric reinforced quartz-based composite material of the present invention has better comprehensive performance by integrally using the hybrid fabric as the reinforcing material. Among these, examples 1 to 3 are preferable embodiments because of their better performance than examples 4 and 5.
TABLE 1
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The utility model provides a fiber mixed fabric reinforcing quartz base combined material, includes reinforcing material and quartz substrate, its characterized in that:
the reinforced material comprises a first outer layer fiber fabric, a core layer fiber fabric and a second outer layer fiber fabric which are sequentially stacked and connected; the first outer layer fiber fabric and the second outer layer fiber fabric are quartz fiber fabrics; the core layer fiber fabric is a carbon fiber and quartz fiber mixed woven fabric or a quartz fiber cloth and carbon fiber cloth mixed woven fabric.
2. The fiber-hybrid fabric-reinforced quartz-based composite material according to claim 1, wherein:
in the reinforced material, the mass ratio of the quartz fiber to the carbon fiber is (95-50%): (5% -50%).
3. The fiber-hybrid fabric-reinforced quartz-based composite material according to claim 1, wherein:
the mass ratio of the carbon fibers to the quartz fibers in the core layer fiber fabric is (100-30%): (0% -70%).
4. The fiber-hybrid fabric-reinforced quartz-based composite material according to claim 1, wherein:
the thickness of the first outer layer fiber fabric is 1-20mm; the thickness of the second outer layer fiber fabric is 1-20mm; the thickness of the core layer fiber fabric is more than or equal to 2mm.
5. A method for preparing the fiber-mixed fabric-reinforced quartz-based composite material according to any one of claims 1 to 4, comprising the steps of:
s1, performing mixed weaving by adopting quartz fibers and carbon fibers, wherein the weaving method is at least one of three-dimensional orthogonal weaving and 2.5D weaving, or performing needling sewing on quartz fiber cloth and carbon fiber cloth to prepare a mixed weaving fiber fabric prefabricated body;
s2, immersing the hybrid fiber fabric prefabricated body by using a solvent, and then drying;
s3, dipping the prefabricated body of the hybrid fiber fabric processed in the step S2 in silica sol;
s4, curing the hybrid fiber fabric prefabricated body soaked with the silica sol to obtain a hybrid fiber reinforced quartz-based composite material intermediate;
and S5, sintering the intermediate of the hybrid fiber reinforced quartz-based composite material to obtain the fiber hybrid fabric reinforced quartz-based composite material.
6. The method of claim 5, wherein:
the step S2 specifically includes: placing the mixed woven fiber fabric prefabricated body into a closed container, vacuumizing the closed container, and then sucking the solvent into the closed container under the vacuum condition to immerse the mixed woven fiber fabric prefabricated body; the solvent is at least one of ethanol and acetone; the immersion treatment conditions were: the pressure is 0-10MPa, the temperature is 60-150 ℃, and the treatment time is 2-24 hours.
7. The method of claim 5, wherein:
in the step S2, the drying temperature is 60-200 ℃, and the drying time is 10-30 hours.
8. The method of claim 5, wherein:
step S3 specifically includes: placing the mixed fiber fabric prefabricated body processed in the step S2 into a closed container, vacuumizing the closed container, and then sucking silica sol into the closed container under a vacuum condition to enable the mixed fiber fabric prefabricated body to be soaked in the silica sol; siO in silica sol 2 The mass concentration of the silica sol is 20 to 80 percent, and the density of the silica sol is 1.00 to 1.65g/cm 3 。
9. The method of claim 5, wherein:
in the step S4, the curing temperature is 100-250 ℃, and the curing time is 24-120h;
in the step S5, the sintering atmosphere is at least one of nitrogen, ammonia and argon or a vacuum environment, the sintering temperature is 300-1000 ℃, and the sintering time is 1-5h.
10. The production method according to claim 5, characterized in that:
further comprising, after step S5: s6, repeating the step S3, the step S4 and the step S5 to 10 times to densify the fiber hybrid fabric reinforced quartz-based composite material.
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| CN116278208A (en) * | 2022-12-20 | 2023-06-23 | 北京玻钢院复合材料有限公司 | Fiber mixed woven fabric reinforced quartz-based composite material and preparation method thereof |
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