CN114315400A - Composite material preparation method based on hot die pressing cracking - Google Patents
Composite material preparation method based on hot die pressing cracking Download PDFInfo
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- CN114315400A CN114315400A CN202210010650.9A CN202210010650A CN114315400A CN 114315400 A CN114315400 A CN 114315400A CN 202210010650 A CN202210010650 A CN 202210010650A CN 114315400 A CN114315400 A CN 114315400A
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000005336 cracking Methods 0.000 title claims abstract description 41
- 238000007723 die pressing method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000000280 densification Methods 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 238000005470 impregnation Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 10
- -1 acryl Chemical group 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229920002554 vinyl polymer Polymers 0.000 claims description 9
- 230000006835 compression Effects 0.000 claims description 7
- 238000007906 compression Methods 0.000 claims description 7
- 229920003257 polycarbosilane Polymers 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 239000011153 ceramic matrix composite Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- 230000001965 increasing effect Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 claims description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000007849 furan resin Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 2
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- 229920001709 polysilazane Polymers 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 229910052796 boron Inorganic materials 0.000 description 4
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
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- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
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Abstract
The invention discloses a preparation method of a composite material based on hot die pressing cracking, which is characterized in that the composite material is subjected to die pressing at a medium temperature (700-1500 ℃) and a medium pressure (1-10 MPa), so that the fiber volume fraction of the composite material is improved, and on the other hand, resin is converted into an inorganic matrix in the heating cracking process, the generated porous matrix is decomposed, is crushed under the action of pressure and is uniformly dispersed into a fiber framework, and the phenomenon that the volume of the porous matrix shrinks to form a blocky structure is avoided. The pressure also reopens some of the closed cells in the matrix resulting from the cracking to facilitate subsequent impregnation. The intermediate-temperature hot-die cracking process is adopted to quickly obtain the intermediate-high density composite material blank in the first period, the densification efficiency is high, the preparation period is greatly shortened, and the preparation cost is obviously reduced. Compared with the existing medium-temperature and high-pressure conditions, the requirements on equipment are greatly reduced, and the preparation and production of large-size and complex-shape engineering samples are easier to realize.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a composite material preparation method based on hot die pressing cracking.
Background
The preparation method of the carbon/carbon composite material and the ceramic matrix composite material mainly comprises a precursor (resin) impregnation-cracking (PIP) process. The precursor (resin) impregnation-cracking process gradually realizes densification through multiple impregnation-cracking. For carbon/carbon composite materials, the existing impregnation-cracking process is mainly an asphalt high-pressure carbonization (HPIC) process, needs medium temperature (700-1000 ℃) and high pressure (80-100MPa), and can realize high density in a short period (2-3), but has strict equipment requirements, high investment and high use cost. For ceramic matrix composites, the PIP process has the problems of low densification efficiency, long preparation period and high cost.
Disclosure of Invention
The invention provides a preparation method of a composite material based on hot die pressing cracking, which is used for overcoming the defects of harsh requirements on equipment, low densification efficiency, long preparation period, high cost and the like in the prior art.
In order to achieve the purpose, the invention provides a preparation method of a composite material based on hot compression cracking, which comprises the following steps:
s1: preparing a fiber prefabricated member by taking fibers and a needled felt as raw materials, and adjusting the content of the fibers in the fiber prefabricated member to be 20-55% by controlling the using amount of the needled felt;
s2: dipping and curing the fiber prefabricated part, and repeating the dipping and curing process for a plurality of times to obtain a cured part;
s3: under inert atmosphere, carrying out hot-die-pressing cracking on the solidified part, and then keeping the pressure of the hot-die-pressing cracking for cooling; the temperature of the hot die pressing cracking is 700-1500 ℃, the pressure is 1-10 MPa, and the pressure is started when the temperature is increased to 500 ℃;
s4: and (5) performing densification treatment on the solidified piece subjected to the step S3 to obtain the composite material.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the preparation method of the composite material based on hot die pressing cracking, the composite material is subjected to die pressing at a medium temperature (700-1500 ℃) and a medium pressure (1-10 MPa), so that the fiber volume fraction of the composite material is improved, and on the other hand, resin is converted into an inorganic matrix in the heating cracking process, the generated porous matrix is decomposed and crushed under the action of pressure and is uniformly dispersed into a fiber framework, and the phenomenon that the volume of the composite material shrinks to form a blocky structure is avoided. The pressure also reopens some of the closed cells in the matrix resulting from the cracking to facilitate subsequent impregnation. The mould pressing compresses the volume of the composite material, so that the volume fraction of the ceramic matrix and the carbon matrix in the composite material is correspondingly increased, namely, a large amount of pores are eliminated by compression, and the microscopic uniformity of the composite material is improved.
2. The composite material preparation method based on hot die pressing cracking provided by the invention can quickly obtain the medium-high density composite material blank in the first period by adopting the medium-temperature hot die pressing cracking process, has high densification efficiency, greatly shortens the preparation period and obviously reduces the preparation cost.
3. Compared with the existing medium-temperature high-pressure conditions, the requirements on equipment are greatly reduced, and the preparation and generation of large-size and complex-shape engineering samples are easier to realize.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides a preparation method of a composite material based on hot die pressing cracking, which comprises the following steps:
s1: the fiber preform is prepared by taking fibers and a needled felt as raw materials, and the content of the fibers in the fiber preform is adjusted to be 20-55% by controlling the using amount of the needled felt.
The fiber prefabricated member is preferably in the structural forms of a needled felt, a fiber cloth and a needled felt, a single fiber laying layer and a needled felt and the like.
Preferably, the content of the fibers in the fiber preform is 20-45%.
Preferably, the content of the fibers in the fiber preform is 20-35%.
In order to fully embody the density increasing effect after hot die pressing cracking, the fiber volume fraction is not too high, and the more suitable fiber volume fraction is 20-45%. Further, the fiber volume fraction is 20-35%.
S2: and carrying out impregnation-solidification on the fiber prefabricated member, and repeating the impregnation-solidification process for a plurality of times to obtain a solidified member.
Preferably, if the composite material is a carbon/carbon composite material, the impregnation liquid for impregnation is one of a phenolic resin solution, a furan resin solution, an epoxy resin solution, an unsaturated polyester resin solution, a cyanate resin solution, and a polyarylacetylene resin solution. When the resin filling is incomplete due to the presence of the solvent, the impregnation-curing step may be repeated, with pressure impregnation-curing being applied as necessary, to fill the voids as completely as possible.
Preferably, if the composite material is a non-oxygen (such as C/SiC) ceramic matrix composite material, the impregnating solution for impregnation is one of a divinylbenzene solution, an acryl-containing polycarbosilane solution, a vinyl-containing polysilane solution, a vinyl-containing polycarbosilane solution, a vinyl-containing polysilazane solution and a vinyl-containing borazane solution of polycarbosilane;
preferably, if the composite material is an oxygen-containing (such as C/SiOC) ceramic matrix composite material, the impregnation liquid for impregnation is one of a methylphenyl silicone resin solution, a vinyl siloxane-containing solution, a divinylbenzene solution of high hydrogen-containing silicone oil, a vinyl siloxane solution and a methylphenyl silicone resin solution.
Preferably, the curing is in particular: 80 ℃/30min, 120-150 ℃/60min and 150-180 ℃/60min to ensure complete curing.
S3: under inert atmosphere, carrying out hot-die-pressing cracking on the solidified part, and then keeping the pressure of the hot-die-pressing cracking for cooling; the temperature of the hot die pressing cracking is 700-1500 ℃, the pressure is 1-10 MPa, and the pressurization is started when the temperature is increased to 500 ℃.
Preferably, the temperature of the hot-pressing cracking is 700-900 ℃, and the pressure is 3-7 MPa.
Considering the effect of compression on densification, the highest pressure is not too low and is generally more than 1.0 MPa; meanwhile, the excessive pressure can cause certain damage to the fiber and is not more than 10.0 MPa. In addition, process parameters that apply too high a pressure also add difficulty to device fabrication. Therefore, a suitable maximum pressurization pressure is 1 to 10MPa, preferably 3 to 7 MPa.
The highest cracking temperature is 700 ℃ to complete inorganic conversion according to the decomposition and conversion temperature of the resin, the temperature of 1500 ℃ or above can collectively generate changes such as crystallization, phase separation, structural rearrangement and the like, and the highest cracking temperature is 700-1500 ℃, preferably 700-900 ℃ in consideration of the technical difficulty of equipment manufacturing.
Preferably, step S3 is specifically:
heating to 500 deg.C from room temperature under nitrogen protection, pressurizing to 0.5MPa when the temperature reaches 500 deg.C, and maintaining;
continuously heating to 600 ℃, pressurizing to 1.5MPa when the temperature reaches 600 ℃, and keeping;
continuously heating to 700 ℃, pressurizing to 2MPa when the temperature reaches 700 ℃, and keeping;
continuously heating to 800 ℃, pressurizing to 3MPa when the temperature reaches 800 ℃, and keeping;
continuously heating to 900 ℃, pressurizing to 5MPa when the temperature reaches 900 ℃, and keeping;
stopping heating, keeping the pressure of 5MPa unchanged, and cooling along with the furnace.
Preferably, step S3 is specifically:
heating to 500 deg.C from room temperature under nitrogen protection, pressurizing to 0.5MPa when the temperature reaches 500 deg.C, and maintaining;
continuously heating to 600 ℃, pressurizing to 1.5MPa when the temperature reaches 600 ℃, and keeping;
continuously heating to 700 ℃, pressurizing to 3MPa when the temperature reaches 700 ℃, and keeping;
continuously heating to 800 ℃, pressurizing to 5MPa when the temperature reaches 800 ℃, and keeping;
continuously heating to 900 ℃, pressurizing to 7MPa when the temperature reaches 900 ℃, and keeping;
stopping heating, keeping the pressure of 5MPa unchanged, and cooling along with the furnace.
S4: and (5) performing densification treatment on the solidified piece subjected to the step S3 to obtain the composite material.
After the first cycle of thermal compression cracking of step S3 is completed, densification is performed using an existing CVI (e.g., J.Am.Ceram.Soc.,80 (1997)) 1897; Carbon,36(1998)1051) or PIP process (e.g., ceramics International,33(2007) 905-. When the PIP process is adopted, the PIP process can be continuously carried out in a hot-die cracking furnace, and the pressure of 0.5-1.0 MPa is applied; or the sample and the mold are fastened with metal beads, screws, etc. prior to cracking to control the sample thickness. The above measures ensure that the thickness of the sample does not change during the subsequent densification process.
Example 1
The embodiment provides a preparation method of a composite material based on hot compression cracking, which comprises the following steps:
s1: the T700 carbon fiber is prepared into needled felt with the volume fraction of the fiber being 28 percent and the size being 220mm multiplied by 25 mm. The fiber preform was subjected to a carbon coating treatment (coating thickness 250nm) on the fiber surface in advance by a CVD process.
S2: vacuum dipping is carried out by adopting a boron phenolic aldehyde/ethanol solution with the concentration of 50%, the boron phenolic aldehyde/ethanol solution is slightly aired, then the boron phenolic aldehyde/ethanol solution is placed in an oven for curing (80 ℃/30min, 120 ℃/60min, 150 ℃/60min), and the dipping-curing process is repeated for 2 times to obtain a cured piece.
S3: and (3) placing the solidified part in a hot die-pressing cracking furnace, and placing a graphite flat plate with the thickness of 250mm multiplied by 35mm on the upper surface and the lower surface of the needled felt respectively as a die. Heating to 500 deg.C from room temperature under nitrogen protection, pressurizing to 0.5MPa when the temperature reaches 500 deg.C, and maintaining;
continuously heating to 600 ℃, pressurizing to 1.5MPa when the temperature reaches 600 ℃, and keeping;
continuously heating to 700 ℃, pressurizing to 2MPa when the temperature reaches 700 ℃, and keeping;
continuously heating to 800 ℃, pressurizing to 3MPa when the temperature reaches 800 ℃, and keeping;
continuously heating to 900 ℃, pressurizing to 5MPa when the temperature reaches 900 ℃, and keeping;
stopping heating, keeping the pressure of 5MPa unchanged, and cooling along with the furnace.
And taking out the sample after cooling and cleaning.
S4: and (5) performing PIP densification treatment on the solidified piece subjected to the step S3 by adopting a boron phenolic aldehyde/ethanol solution to obtain the composite material.
The C/C composite material prepared in the example is detected to have the thickness of 14.3mm and the density of 1.45g/cm3。
Example 2
The embodiment provides a preparation method of a composite material based on hot compression cracking, which comprises the following steps:
s1: the same as in example 1.
S2: the preparation method comprises the steps of adopting polycarbosilane/divinylbenzene (the weight ratio is 1:1, chloroplatinic acid/ethanol solution with the polycarbosilane weight ratio of 20ppm (mg/L) (indicating platinum content) is added as a catalyst) solution for vacuum impregnation, slightly airing, placing in an oven for curing (80 ℃/30min, 150 ℃/60min, 180 ℃/60min), and repeating the impregnation-curing process for 2 times to obtain a cured part.
S3: and (3) placing the solidified part in a hot die-pressing cracking furnace, and placing a flat plate of 250mm multiplied by 35mm on the upper surface and the lower surface of the needled felt respectively as a die. Heating to 500 deg.C from room temperature under nitrogen protection, pressurizing to 0.5MPa when the temperature reaches 500 deg.C, and maintaining;
continuously heating to 600 ℃, pressurizing to 1.5MPa when the temperature reaches 600 ℃, and keeping;
continuously heating to 700 ℃, pressurizing to 3MPa when the temperature reaches 700 ℃, and keeping;
continuously heating to 800 ℃, pressurizing to 5MPa when the temperature reaches 800 ℃, and keeping;
continuously heating to 900 ℃, pressurizing to 7MPa when the temperature reaches 900 ℃, and keeping;
stopping heating, keeping the pressure of 5MPa unchanged, and cooling along with the furnace.
S4: the same as in example 1.
The C/SiC composite material prepared in the example is detected to have the thickness of 12.6mm and the density of 1.53g/cm3。
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of a composite material based on hot compression cracking is characterized by comprising the following steps:
s1: preparing a fiber prefabricated member by taking fibers and a needled felt as raw materials, and adjusting the content of the fibers in the fiber prefabricated member to be 20-55% by controlling the using amount of the needled felt;
s2: dipping and curing the fiber prefabricated part, and repeating the dipping and curing process for a plurality of times to obtain a cured part;
s3: under inert atmosphere, carrying out hot-die-pressing cracking on the solidified part, and then keeping the pressure of the hot-die-pressing cracking for cooling; the temperature of the hot die pressing cracking is 700-1500 ℃, the pressure is 1-10 MPa, and the pressure is started when the temperature is increased to 500 ℃;
s4: and (5) performing densification treatment on the solidified piece subjected to the step S3 to obtain the composite material.
2. The method of claim 1, wherein in step S1, the fiber content of the fiber preform is 20-45%.
3. The method for preparing a composite material according to claim 1 or 2, wherein the content of the fibers in the fiber preform is 20 to 35%.
4. The method of preparing a composite material according to claim 1, wherein in step S2, if the composite material is a carbon/carbon composite material, the impregnating solution is one of a phenol resin solution, a furan resin solution, an epoxy resin solution, an unsaturated polyester resin solution, a cyanate resin solution, and a polyarylacetylene resin solution.
5. The method of claim 1, wherein in step S2, if the composite material is a non-oxygen-containing ceramic matrix composite material, the impregnating solution is one of a divinylbenzene solution of polycarbosilane, an acryl-containing polycarbosilane solution, a vinyl-containing polysilane solution, a vinyl-containing polysilazane solution, and a vinyl-containing borazane solution.
6. The method according to claim 1, wherein in step S2, if the composite material is an oxygen-containing ceramic matrix composite material, the impregnation liquid is one of a methylphenylsilicone resin solution, a vinylsiloxane solution, a divinylbenzene solution of high hydrogen-containing silicone oil, a vinylsiloxane solution, and a methylphenylsilicone resin solution.
7. The method for preparing a composite material according to claim 1, wherein in step S2, the curing is specifically: 80 ℃/30min, 120-150 ℃/60min, 150-180 ℃/60 min.
8. The method for preparing a composite material according to claim 1, wherein in step S3, the temperature of the hot-mold cracking is 700 to 900 ℃ and the pressure is 3 to 7 MPa.
9. The method for preparing a composite material according to claim 1, wherein the step S3 specifically comprises:
heating to 500 deg.C from room temperature under nitrogen protection, pressurizing to 0.5MPa when the temperature reaches 500 deg.C, and maintaining;
continuously heating to 600 ℃, pressurizing to 1.5MPa when the temperature reaches 600 ℃, and keeping;
continuously heating to 700 ℃, pressurizing to 2MPa when the temperature reaches 700 ℃, and keeping;
continuously heating to 800 ℃, pressurizing to 3MPa when the temperature reaches 800 ℃, and keeping;
continuously heating to 900 ℃, pressurizing to 5MPa when the temperature reaches 900 ℃, and keeping;
stopping heating, keeping the pressure of 5MPa unchanged, and cooling along with the furnace.
10. The method for preparing a composite material according to claim 1, wherein the step S3 specifically comprises:
heating to 500 deg.C from room temperature under nitrogen protection, pressurizing to 0.5MPa when the temperature reaches 500 deg.C, and maintaining;
continuously heating to 600 ℃, pressurizing to 1.5MPa when the temperature reaches 600 ℃, and keeping;
continuously heating to 700 ℃, pressurizing to 3MPa when the temperature reaches 700 ℃, and keeping;
continuously heating to 800 ℃, pressurizing to 5MPa when the temperature reaches 800 ℃, and keeping;
continuously heating to 900 ℃, pressurizing to 7MPa when the temperature reaches 900 ℃, and keeping;
stopping heating, keeping the pressure of 5MPa unchanged, and cooling along with the furnace.
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2022
- 2022-01-05 CN CN202210010650.9A patent/CN114315400A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2002068362A1 (en) * | 2001-02-27 | 2002-09-06 | Japan Science And Technology Corporation | Method for producing sic fiber-reinforced sic composite material having excellent fracture toughness |
| CN102276279A (en) * | 2011-06-10 | 2011-12-14 | 中国人民解放军国防科学技术大学 | Preparation method of silicon carbide fiber reinforced silicon carbide composite material |
| US20180335099A1 (en) * | 2017-05-16 | 2018-11-22 | Goodrich Corporation | Rapid ceramic matrix composite fabrication of aircraft brakes via field assisted sintering |
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