CN116606522B - Quartz fiber prepreg and preparation method and application thereof - Google Patents
Quartz fiber prepreg and preparation method and application thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 121
- 239000010453 quartz Substances 0.000 title claims abstract description 79
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 38
- 239000002131 composite material Substances 0.000 claims abstract description 33
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 24
- 230000001678 irradiating effect Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 4
- 230000008569 process Effects 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 239000005011 phenolic resin Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 238000007731 hot pressing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 239000009719 polyimide resin Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 40
- 239000000243 solution Substances 0.000 description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 7
- 230000005855 radiation Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- VQNDBXJTIJKJPV-UHFFFAOYSA-N 2h-triazolo[4,5-b]pyridine Chemical compound C1=CC=NC2=NNN=C21 VQNDBXJTIJKJPV-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- -1 hexafluorophosphate Chemical compound 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/246—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using polymer based synthetic fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/247—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using fibres of at least two types
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/248—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using pre-treated fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/40—Weight reduction
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- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a quartz fiber prepreg, a preparation method and application thereof, wherein the prepreg is prepared from the following raw materials in percentage by weight: 25% -45% of a resin system; 55% -75% of reinforcing fibers; wherein the reinforcing fiber comprises the following components in percentage by mass (1-3): the graphene grafted quartz fiber and the modified PBO fiber of (1-5): the modified PBO fiber is PBO fiber subjected to ultraviolet irradiation treatment, and the specific treatment process is as follows: and (3) irradiating the PBO fiber subjected to cleaning and drying with ultraviolet light for 10-60 seconds, and then raising the temperature to 150-160 ℃ at 2-8 ℃/min, and keeping the temperature for 2-4 hours. The composite material disclosed by the invention can resist high temperature of more than 1800 ℃, can meet the comprehensive performance of an ultra-high sound velocity aircraft in a special service environment, and has a wide application prospect in the fields of aviation, aerospace, nuclear energy and the like.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a quartz fiber prepreg and a preparation method and application thereof.
Background
The thermal protection material has special use environment, the highest temperature of the outer surface of the material reaches 1500-2000 ℃ and the temperature of the inner surface does not exceed 150 ℃ in the service process, and a remarkable large temperature gradient exists. The space motor aircraft runs and executes tasks on orbit for more than one year, the heat protection material covers the whole aircraft surface, so that the highest temperature of the parts such as the head/the front edge of the wing is more than 1800 ℃, the large area of the windward is more than 1500 ℃, the severe requirements are put on the temperature resistance of the heat protection system, in addition, the lightening of the heat protection material is not only an important way for improving the effective load of the aircraft, but also can determine the feasibility of the design of the aircraft. However, none of the existing heat insulating materials can meet the above requirements.
Therefore, the development of the thermal protection composite material integrating the comprehensive properties of high efficiency, heat insulation, light weight, reliability, repeated use and the like has important application significance.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects in the prior art, and proposes a quartz fiber prepreg, and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a quartz fiber prepreg prepared from the following raw materials in percentage by weight:
25% -45% of a resin system;
55% -75% of reinforcing fibers;
wherein the reinforcing fiber comprises the following components in percentage by mass (1-3): the graphene grafted quartz fiber and the modified PBO fiber of (1-5):
the modified PBO fiber is PBO fiber subjected to ultraviolet irradiation treatment, and the specific treatment process is as follows: and (3) irradiating the PBO fiber subjected to cleaning and drying with ultraviolet light for 10-60 seconds, and then raising the temperature to 150-160 ℃ at 2-8 ℃/min, and keeping the temperature for 2-4 hours.
Preferably, the preparation method of the graphene grafted quartz fiber comprises the following steps: and adding 0.005-0.008 weight part of condensing agent and 2-5 weight parts of quartz fiber into the graphene oxide dispersion liquid, stirring for 2-6 hours, washing 3-8 times by using a solvent, and drying the product to obtain the graphene grafted quartz fiber.
More preferably, in the preparation method of the graphene grafted quartz fiber, the mass ratio of graphene oxide to condensing agent to quartz fiber is (4-6): (0.005-0.008): (2-5).
More preferably, in the preparation method of the graphene grafted quartz fiber, the mass ratio of graphene oxide to condensing agent to quartz fiber is 4:0.008:5.
preferably, the condensing agent is 2- (7-azabenzotriazol) -N, N' -tetramethylurea hexafluorophosphate.
Preferably, the solvent is N, N-dimethylformamide.
Preferably, the resin system is one or a mixture of more than two of polyimide resin, phenolic resin, epoxy resin and organic silicon resin.
The invention also provides a preparation method of the quartz fiber prepreg, which comprises the following steps:
s1: mixing and dissolving a resin system and an organic solvent to obtain a uniform resin precursor solution;
s2: and mixing the resin precursor solution with the reinforcing fibers to remove the organic solvent, thereby obtaining the quartz fiber prepreg.
The invention further provides a composite material prepared from the quartz fiber prepreg, and the preparation method of the composite material comprises the following steps: and (3) alternately layering the quartz fiber prepreg, and performing hot pressing curing treatment to obtain the composite material.
The invention further provides application of the composite material in preparing a heat protection material in the aerospace industry field or the civil industry field.
Compared with the prior art, the invention has the following advantages:
(1) According to the invention, the PBO fiber or the quartz fiber added into the matrix can reduce the thermal stress, obviously improve the crack propagation resistance and the thermal shock resistance of the material, change the breaking mode of the material from brittle fracture to non-brittle fracture, and improve the thermal shock resistance, damage tolerance and reliability of the material under a severe heating environment.
(2) According to the invention, the surface of the PBO fiber is modified by ultraviolet irradiation, and the ultraviolet irradiation parameters are reasonably controlled, so that the heat resistance of the PBO fiber is improved, and the performances of high temperature resistance, shrinkage resistance, oxidation resistance, thermal shock resistance and the like of the composite material are improved by the combined action of the PBO fiber and the graphene grafted quartz fiber.
(3) According to the prepreg, the graphene, the quartz fiber and the PBO fiber are matched to increase the heat radiation coefficient of the composite material, so that the composite material forms a heat radiation heat shield, and the radiation resistance and heat insulation effects are improved.
(4) The composite material disclosed by the invention can resist high temperature of more than 1800 ℃, can meet the comprehensive performance of an ultra-high sound velocity aircraft in a special service environment, and has a wide application prospect in the fields of aviation, aerospace, nuclear energy and the like.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the inventive concepts pertain. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
(1) Preparation of graphene grafted quartz fiber
To an aqueous solution containing 4 parts by weight of graphene oxide dispersion (the graphene oxide dispersion in this example is a commercially available aqueous solution of graphene oxide, the same applies hereinafter), 0.008 parts by weight of a condensing agent (2- (7-azabenzotriazol) -N, N' -tetramethylurea hexafluorophosphate, the same applies hereinafter) and 5 parts by weight of quartz fiber were added, and the mixture was stirred for 6 hours, washed 8 times with N, N-dimethylformamide, and the resultant was dried to obtain graphene-grafted quartz fiber.
(2) Preparation of modified PBO fibers
The PBO fiber has the ultraviolet light wavelength of 313 nm and the irradiation intensity of 750W/m 2 Respectively irradiating for 50 seconds, and then taking out to obtain the modified PBO fiber.
(3) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 25 parts by weight of phenolic resin and 100 parts by weight of n-hexane to obtain a uniform resin precursor solution;
s2: mixing the resin precursor solution with 75 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber comprises the following components in percentage by mass: 2 and modified PBO fibers.
(4) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Example 2
(1) Preparation of graphene grafted quartz fiber
To a dispersion containing 5 parts by weight of graphene oxide, 0.005 parts by weight of a condensing agent and 3 parts by weight of a quartz fiber were added, stirred for 6 hours, washed 8 times with N, N-dimethylformamide, and the product was dried to obtain a graphene grafted quartz fiber.
(2) Preparation of modified PBO fibers
The PBO fiber has the ultraviolet light wavelength of 313 nm and the irradiation intensity of 750W/m 2 And respectively irradiating for 50 seconds under the condition, and taking out to obtain the modified PBO fiber.
(3) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 30 parts by weight of phenolic resin and 150 parts by weight of n-hexane to obtain a uniform resin precursor solution;
s2: mixing the resin precursor solution with 70 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber comprises the following components in percentage by mass: 3 and modified PBO fibers.
(4) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Example 3
(1) Preparation of graphene grafted quartz fiber
To a dispersion containing 6 parts by weight of graphene oxide, 0.005 parts by weight of a condensing agent and 2 parts by weight of a quartz fiber were added, stirred for 6 hours, washed 8 times with N, N-dimethylformamide, and the product was dried to obtain a graphene grafted quartz fiber.
(2) Preparation of modified PBO fibers
The PBO fiber has the ultraviolet light wavelength of 313 nm and the irradiation intensity of 750W/m 2 And respectively irradiating for 50 seconds under the condition, and taking out to obtain the modified PBO fiber.
(3) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 40 parts by weight of phenolic resin and 180 parts by weight of normal hexane to obtain a uniform resin precursor solution;
s2: mixing the resin precursor solution with 60 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber comprises the following components in percentage by mass: 1 and modified PBO fibers.
(4) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Example 4
(1) Preparation of graphene grafted quartz fiber
To a dispersion containing 4 parts by weight of graphene oxide, 0.007 parts by weight of a condensing agent and 5 parts by weight of quartz fiber were added, stirred for 6 hours, washed 8 times with N, N-dimethylformamide, and the product was dried to obtain graphene grafted quartz fiber.
(2) Preparation of modified PBO fibers
The PBO fiber has the ultraviolet light wavelength of 313 nm and the irradiation intensity of 750W/m 2 And respectively irradiating for 50 seconds under the condition, and taking out to obtain the modified PBO fiber.
(3) Preparation of a Quartz fiber prepreg
S1: mixing 45 parts by weight of phenolic resin with 200 parts by weight of n-hexane and dissolving to obtain a uniform resin precursor solution;
s2: mixing the resin precursor solution with 55 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber comprises the following components in percentage by mass: 5 and modified PBO fibers.
(4) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Comparative example 1
(1) Preparation of modified PBO fibers
The PBO fiber has the ultraviolet light wavelength of 313 nm and the irradiation intensity of 750W/m 2 And respectively irradiating for 50 seconds under the condition, and taking out to obtain the modified PBO fiber.
(2) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 25 parts by weight of phenolic resin and 100 parts by weight of n-hexane to obtain a uniform resin precursor solution;
s2: mixing the resin precursor solution with 75 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber comprises the following components in percentage by mass: 2 and modified PBO fibers.
(3) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Comparative example 2
(1) Preparation of graphene grafted quartz fiber
To a dispersion containing 4 parts by weight of graphene oxide, 0.008 parts by weight of a condensing agent and 5 parts by weight of a quartz fiber were added, stirred for 6 hours, washed 8 times with N, N-dimethylformamide, and the product was dried to obtain a graphene grafted quartz fiber.
(2) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 25 parts by weight of phenolic resin and 100 parts by weight of n-hexane to obtain a uniform resin precursor solution;
s2: mixing the resin precursor solution with 75 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber comprises the following components in percentage by mass: 2 and PBO fibers.
(3) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Comparative example 3
(1) Preparation of graphene grafted quartz fiber
To a dispersion containing 4 parts by weight of graphene oxide, 0.008 parts by weight of a condensing agent and 5 parts by weight of a quartz fiber were added, stirred for 6 hours, washed 8 times with N, N-dimethylformamide, and the product was dried to obtain a graphene grafted quartz fiber.
(2) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 25 parts by weight of phenolic resin and 100 parts by weight of n-hexane to obtain a uniform resin precursor solution;
s2: and mixing the resin precursor solution with 75 parts by weight of reinforcing fiber to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fiber is graphene grafted quartz fiber.
(3) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Comparative example 4
(1) Preparation of modified PBO fibers
The PBO fiber has the ultraviolet light wavelength of 313 nm and the irradiation intensity of 750W/m 2 And respectively irradiating for 50 seconds under the condition, and taking out to obtain the modified PBO fiber.
(2) Preparation of a Quartz fiber prepreg
S1: mixing and dissolving 25 parts by weight of phenolic resin and 100 parts by weight of n-hexane to obtain a uniform resin precursor solution;
s2: and mixing the resin precursor solution with 75 parts by weight of reinforcing fibers to remove the organic solvent to obtain the quartz fiber prepreg with the thickness of 5mm, wherein the reinforcing fibers are modified PBO fibers.
(3) Preparation of composite materials
Alternately layering the prepared quartz fiber prepreg until the total thickness is 25mm, and performing hot press curing on the alternately layered prepreg, wherein the parameters of the hot press curing are as follows: the pressure is 12MPa, and the composite material is finally prepared by sequentially carrying out heat preservation and pressure maintaining for 1h at 60 ℃, heat preservation and pressure maintaining for 1h at 100 ℃, heat preservation and pressure maintaining for 2h at 120 ℃, heat preservation and pressure maintaining for 2h at 150 ℃ and heat preservation and pressure maintaining for 2h at 200 ℃.
Test case
Measuring the heat conductivity coefficient of the material at 1800 ℃ by adopting an LFA 427 heat conductivity tester; measuring the heat conductivity coefficient of the material at 24 ℃ by adopting a TC3000 heat conductivity coefficient meter; compressive strength at 24℃and 1800℃of the composite materials prepared in examples 1 to 4 and comparative examples 1 to 4 were measured by using a Teller 1800℃high temperature tensile tester, and linear shrinkage of the materials after 1800℃for 1 hour was measured at 24℃and the results are shown in Table 1.
TABLE 1 Performance test results of the composite materials prepared in examples 1-4 and comparative examples 1-4
The performance tests of the examples 1-4 and the comparative examples 1-4 show that the composite material prepared by the scheme of the invention can keep higher strength and lower heat conductivity coefficient at normal temperature and high temperature of 1800 ℃ and has higher comprehensive performance.
The above embodiments are merely preferred embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A quartz fiber prepreg, characterized in that: the prepreg is prepared from the following raw materials in percentage by weight:
25% -45% of a resin system;
55% -75% of reinforcing fibers;
wherein the reinforcing fiber comprises the following components in percentage by mass (1-3): the graphene grafted quartz fiber and the modified PBO fiber of (1-5):
the modified PBO fiber is PBO fiber subjected to ultraviolet irradiation treatment, and the specific treatment process is as follows: irradiating the cleaned and dried PBO fiber with ultraviolet light for 10-60 seconds, and then raising the temperature to 150-160 ℃ at 2-8 ℃/min, and keeping for 2-4 hours;
the preparation method of the graphene grafted quartz fiber comprises the following steps: adding a condensing agent and quartz fibers into the graphene oxide dispersion liquid, stirring for 2-6 hours, washing for 3-8 times by using a solvent, and drying the product to obtain graphene grafted quartz fibers; wherein, the mass ratio of graphene oxide, condensing agent and quartz fiber is (4-6): (0.005-0.008): (2-5); the condensing agent is 2- (7-aza-benzotriazol) -N, N, N ', N' -tetramethyl urea hexafluorophosphate.
2. The quartz fiber prepreg of claim 1, wherein: in the preparation method of the graphene grafted quartz fiber, the mass ratio of graphene oxide to condensing agent to quartz fiber is 4:0.008:5.
3. the quartz fiber prepreg of claim 1, wherein: the solvent is N, N-dimethylformamide.
4. The quartz fiber prepreg of claim 1, wherein: the resin system is one or a mixture of more than two of polyimide resin, phenolic resin, epoxy resin and organic silicon resin.
5. A method for producing a quartz fiber prepreg according to any one of claims 1-4, characterized in that: the preparation method comprises the following steps:
s1: mixing and dissolving a resin system and an organic solvent to obtain a uniform resin precursor solution;
s2: and mixing the resin precursor solution with the reinforcing fibers to remove the organic solvent, thereby obtaining the quartz fiber prepreg.
6. A composite material characterized by: the composite material is obtained by alternately layering the quartz fiber prepreg according to any one of claims 1-4 and then performing hot pressing curing treatment.
7. Use of the composite material of claim 6 for the preparation of a thermal protection material in the aerospace industry or civil industry.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105113073A (en) * | 2015-07-20 | 2015-12-02 | 湖北菲利华石英玻璃股份有限公司 | Production method for quartz fiber blended yarns |
| CN107723830A (en) * | 2017-11-03 | 2018-02-23 | 中科纺织研究院（青岛）有限公司 | A kind of preparation method and application of high-tenacity graphene oxide grafting nylon fibre |
| CN111574808A (en) * | 2020-04-29 | 2020-08-25 | 航天材料及工艺研究所 | Light heat-insulating composite material and preparation method thereof |
| CN113445309A (en) * | 2020-03-25 | 2021-09-28 | 赣州西维尔金属材料科技有限公司 | Conductive PBO fiber and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105113073A (en) * | 2015-07-20 | 2015-12-02 | 湖北菲利华石英玻璃股份有限公司 | Production method for quartz fiber blended yarns |
| CN107723830A (en) * | 2017-11-03 | 2018-02-23 | 中科纺织研究院（青岛）有限公司 | A kind of preparation method and application of high-tenacity graphene oxide grafting nylon fibre |
| CN113445309A (en) * | 2020-03-25 | 2021-09-28 | 赣州西维尔金属材料科技有限公司 | Conductive PBO fiber and preparation method thereof |
| CN111574808A (en) * | 2020-04-29 | 2020-08-25 | 航天材料及工艺研究所 | Light heat-insulating composite material and preparation method thereof |
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