CN117602954A - Carbon-based composite material separated by continuous silicon carbide ceramic framework, and preparation method and application thereof - Google Patents
Carbon-based composite material separated by continuous silicon carbide ceramic framework, and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 239000002131 composite material Substances 0.000 title claims abstract description 98
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 78
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 72
- 239000000919 ceramic Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 26
- 230000003647 oxidation Effects 0.000 claims abstract description 25
- 239000011159 matrix material Substances 0.000 claims abstract description 21
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 17
- 238000005049 combustion synthesis Methods 0.000 claims abstract description 15
- 239000002931 mesocarbon microbead Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 40
- 239000004005 microsphere Substances 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000011863 silicon-based powder Substances 0.000 claims description 11
- 238000002490 spark plasma sintering Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 238000005452 bending Methods 0.000 claims description 5
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000008569 process Effects 0.000 abstract description 19
- 238000005253 cladding Methods 0.000 abstract 2
- 229910002804 graphite Inorganic materials 0.000 description 39
- 239000010439 graphite Substances 0.000 description 39
- 239000012071 phase Substances 0.000 description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
- 239000011812 mixed powder Substances 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000000498 ball milling Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 239000000376 reactant Substances 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 239000011325 microbead Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- IWBUYGUPYWKAMK-UHFFFAOYSA-N [AlH3].[N] Chemical compound [AlH3].[N] IWBUYGUPYWKAMK-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000005475 siliconizing Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention discloses a carbon-based composite material separated by continuous silicon carbide ceramics, a preparation method and application thereof, and belongs to the technical field of inorganic nonmetallic material preparation. According to the invention, the mesocarbon microbeads are used as matrix phase, silicon carbide is used as ceramic reinforcing phase, and the ceramic reinforcing phase tightly surrounds the matrix phase to form the isotropic structure composite material with continuous reinforcing phase and separated matrix phase. Firstly, a silicon carbide layer is generated on the surface of the mesocarbon microbead in situ by a combustion synthesis method to form cladding powder, and then the cladding powder is sintered to form the continuous silicon carbide ceramic separated carbon-based composite material. The preparation method of the carbon-based composite material separated by the silicon carbide ceramic has the advantages of stable process and low cost, and the prepared isotropic carbon-based composite material with excellent sintering property, mechanical property and oxidation resistance can meet the application requirements in the fields of nuclear industry, aerospace and the like, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic material preparation, and particularly relates to a carbon-based composite material separated by continuous silicon carbide ceramics, and a preparation method and application thereof.
Background
Nuclear graphite is used as a structural material and a moderator of a high temperature gas cooled reactor due to its excellent neutron moderating ability, irradiation resistance and good high temperature stability. However, in the novel air-cooled micro-stack using air as a cooling medium, graphite material of the core reacts with oxidizing gas under high temperature condition (> 773K) to cause oxidation corrosion, thereby reducing mechanical and thermal properties of graphite and affecting service life of graphite members. The preparation of an oxidation-resistant ceramic coating on the surface of graphite is a common method for improving oxidation resistance and also achieves better effects [ inorganic materials theory, 2007,22 (4): 737-741 ]. However, due to the difference in thermal expansion coefficients of the coating and the matrix, once the coating is damaged by oxidation corrosion, the graphite matrix will rapidly oxidize, limiting the long-term use of graphite in high temperature oxygen environments. Therefore, the development of a novel nuclear graphite material which can be reliably used for a long time in a high-temperature oxygen-containing atmosphere has important strategic significance and practical value.
To overcome the above problems, researchers have attempted to develop ceramic reinforced graphite-based composite materials. For example, japanese eastern carbon researchers [ J.Eur.Ceram.Soc.,2014,34 (3): 837-840 ] prepared continuous reticular silicon carbide ceramic reinforced graphite composite material by using isotropic graphite powder and silicon nitride powder as raw materials and adopting a gel casting and reaction sintering process, found that the material only has surface oxidation after being oxidized for 10 hours in the air at 600 ℃, and the oxidation resistance of a graphite matrix is improved to a certain extent, but the oxidation reaction is not well inhibited because partial pores still exist in the SiC skeleton in the material. Researches (Ceram. Int.,2013, 39:81-86.) are carried out on the intermediate phase carbon microsphere green compact to carry out liquid phase siliconizing to prepare a compact reticular silicon carbide ceramic reinforced graphite composite material, and the formed compact silicon carbide ceramic skeleton separates and protects intermediate phase carbon microsphere particles, thereby improving the anti-ablative performance of the intermediate phase carbon microsphere green compact. However, due to the limitation of the preparation method, the silicon carbide ceramic skeleton of the composite material cannot completely and independently separate and protect the mesophase carbon microsphere particles, so that the oxidation separation inhibition effect of the ceramic skeleton cannot be fully exerted. From the above, the graphite matrix is separated and protected by using the continuous oxidation-resistant ceramic as the reinforcing phase through reasonable microstructure design and effective preparation method, which is an effective method for realizing the long-acting oxidation resistance of the nuclear graphite material. The silicon carbide layer is coated on the surface of the mesocarbon microbead by a molten salt method, and then the silicon carbide reinforced carbon-based composite material is successfully prepared by hot-pressing sintering, so that the mechanical property of the composite material can be improved to a certain extent [ a silicon carbide reinforced carbon-based composite material and a preparation method, chinese patent invention, ZL201910198813.9 ]. However, the lower reaction temperature of the molten salt method limits the increase of the thickness of the silicon carbide layer which is dominant by diffusion, the continuity of the ceramic reinforcing phase is poor, and the improvement of the oxidation resistance of the composite material is not obvious. The ceramic reinforced graphite-based composite material prepared by directly ball-milling and mixing ceramic and graphite powder and then sintering can accurately regulate and control the content of the reinforced phase, but agglomeration of graphite particles cannot be avoided, and the combination property between the ceramic and the graphite is poor. Thus, how to ensure ceramic reinforcement with respect to the separation of the graphite matrix and good interface bonding of the ceramic/graphite has been a great challenge and challenge.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a carbon-based composite material separated by continuous silicon carbide ceramics, and a preparation method and application thereof, so as to solve the technical problems that graphite matrix in the existing graphite-based composite material is easy to agglomerate and has low bonding strength with ceramic reinforcement.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention discloses a carbon-based composite material separated by continuous silicon carbide ceramics, which takes mesocarbon microbeads as matrix phase and silicon carbide as ceramic reinforcing phase, wherein the ceramic reinforcing phase tightly surrounds the matrix phase to form an isotropic structure composite material with continuous reinforcing phase and separated matrix phase; wherein, the composite material comprises 50-90% of mesophase carbon microspheres and 10-50% of silicon carbide ceramics by volume percent.
Preferably, the relative density of the composite material is 91.13% -99.27%; the apparent porosity is 0.23 to 6.38 percent; the bending strength is 92-325 MPa, and the mass loss of oxidation in air at 900 ℃ for 1 hour is 2.5-6.3%.
The invention also discloses a preparation method of the continuous silicon carbide ceramic separated carbon-based composite material, which comprises the following steps:
1) Silicon powder and mesophase carbon microspheres are used as raw materials, polytetrafluoroethylene is used as a reaction promoter, aluminum powder and aluminum nitride powder are used as composite ignition agents, and the raw materials and the reaction promoter are fully and uniformly mixed to obtain reaction raw material powder;
2) And (3) prepressing and forming the reaction raw material powder to obtain a prepressing and forming sample, embedding the prepressing and forming sample into a composite ignition agent, performing combustion synthesis under nitrogen atmosphere, and cooling to obtain the coating powder of the silicon carbide coated mesophase carbon microsphere.
3) Taking the coated powder as a sintering raw material, taking aluminum oxide and yttrium oxide as a composite sintering auxiliary agent, and fully and uniformly mixing the sintering raw material and the composite sintering auxiliary agent to obtain powder to be sintered;
4) And (3) carrying out spark plasma sintering on the powder to be sintered at 1500-1800 ℃, and carrying out cooling treatment after heat preservation to prepare the carbon-based composite material separated by the continuous silicon carbide ceramic.
Preferably, in the step 1), the mole ratio of the silicon powder to the mesocarbon microbeads is 1 (3-20); the mass ratio of the aluminum powder to the aluminum nitride powder is 1:1; the mass ratio of the reaction accelerator to the raw materials is 1 (5-20).
Preferably, in the step 1), fully and uniformly mixing, ball milling is carried out, mixed powder of raw materials and a reaction promoter is put into a planetary ball milling tank, the mass ratio of agate grinding balls to the mixed powder is 5:1, and the added liquid ball milling medium is absolute ethyl alcohol, and the mass ratio of the absolute ethyl alcohol to the mixed powder is 1:1; after sealing, ball milling is carried out for 2 hours at a rotating speed of 200 revolutions per minute, thus obtaining uniform reaction raw material slurry, and the reaction raw material powder is obtained after drying and sieving.
Preferably, in step 1), the mesophase carbon microbeads used have a particle size of 8-12 μm; the grain diameter of the polytetrafluoroethylene is 5-10 mu m, and the purity is more than 99.9%; the grain diameter range of the used silicon powder is 1-3 mu m, and the purity is more than 99.0 percent; the grain diameter range of the aluminum powder is 3-5 mu m, and the purity is more than 99.9%; the grain size range of the aluminum nitride is 3-5 mu m, and the purity is more than 99.99%.
Preferably, in the step 2), the pressure of the pre-pressing molding is 30MPa, and the pressure is maintained for 2 minutes.
Preferably, in the step 2), the pressure of the nitrogen atmosphere is 0.5-3 MPa, and the purity is 99.99%; the current-carrying voltage for combustion synthesis was 20V, the current-carrying current was 60A, and the current-carrying time was 40 seconds.
Preferably, in step 3), the alumina powder used has a particle size ranging from 0.5 to 3 μm and a purity of greater than 99.9%; the grain diameter range of the yttrium oxide powder is 0.5-3 mu m, and the purity is more than 99.99%; the mol ratio of the alumina powder to the yttrium oxide powder is 5:3; the mass ratio of the composite sintering aid to the sintering raw material is 1 (10-30).
Preferably, in the step 3), fully and uniformly mixing, ball milling is adopted, mixed powder of raw materials and a composite sintering additive is put into a planetary ball milling tank, the mass ratio of agate grinding balls to the mixed powder is 5:1, and the added liquid ball milling medium is absolute ethyl alcohol, and the mass ratio of the absolute ethyl alcohol to the mixed powder is 1:1; after sealing, ball milling is carried out for 2 hours at the rotating speed of 200 revolutions per minute, thus obtaining uniform sintering raw material slurry, and drying and sieving are carried out, thus obtaining sintering raw material powder.
Preferably, in the step 4), spark plasma sintering is performed by applying an axial pressure of 30 to 70MPa to the pre-press-molded sample under vacuum or under a protective atmosphere, and activating the sample with a pulse current for 60 seconds.
Preferably, in the step 4), the temperature system of the heat preservation treatment is divided into three stages, wherein the first stage is heated to 1000 ℃ from room temperature at a heating rate of 200-300 ℃/min, the second stage is heated to 1400 ℃ from 1000 ℃ at a heating rate of 150-200 ℃/min, and the third stage is heated to the final sintering temperature from 1400 ℃ at a heating rate of 100-150 ℃/min; the heat preservation time is 5 minutes.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a carbon-based composite material separated by continuous silicon carbide ceramics, which takes micron-sized silicon powder and mesophase carbon microspheres as raw materials, forms a silicon carbide layer with uniform thickness and controllable thickness on the surface of the mesophase carbon microspheres through combustion synthesis in-situ reaction, and takes the mesophase carbon microspheres coated by silicon carbide as a sintering raw material for spark plasma sintering, wherein the silicon carbide ceramics are sintered and densified in the process to form a continuous isotropic structure, thus the technical problems of agglomeration of graphite matrix phase and low bonding strength with ceramic reinforcement can be effectively solved, and the applicability is obviously improved. The nano silicon carbide formed by combustion synthesis can overcome the defect that graphite is difficult to compact, and the silicon carbide ceramic is tightly combined with the mesophase carbon microsphere, so that the high-strength characteristic is provided for the composite material. The continuous silicon carbide ceramic reinforced phase separates and protects the graphite matrix phases from each other, and prevents oxidizing gas from penetrating into the composite material, so that the composite material has good oxidation resistance.
The preparation method of the carbon-based composite material separated by the continuous silicon carbide ceramic has the following advantages:
firstly, by utilizing the characteristic of rapid reaction and high temperature of a combustion synthesis method, the continuous proceeding of the aluminum nitrogen combustion reaction and the polytetrafluoroethylene reaction accelerator auxiliary silicon carbon combustion reaction can ensure that silicon carbide can be generated on the surface of the mesocarbon microbeads in situ, thereby enhancing the bonding strength of the silicon carbide and the mesocarbon microbeads and ensuring the uniformity degree of the formation of the silicon carbide on the surfaces of the carbon microbeads. Meanwhile, the content of the silicon carbide reinforcing phase can be regulated and controlled by directly regulating the proportion of the silicon powder and the mesocarbon microbeads.
Secondly, the submicron silicon carbide formed by combustion synthesis has excellent sintering performance, and the defect that graphite is difficult to compact can be overcome; and the silicon carbide ceramic skeleton formed by sintering is tightly combined with the mesophase carbon microsphere, so that the mechanical property of the composite material is greatly enhanced.
Thirdly, each mesocarbon microbead is independently separated and combined by the continuous silicon carbide ceramic reinforcing phase, so that the effect of blocking an oxygen diffusion path is achieved, and the oxidation resistance of the mesocarbon microbead is improved. The evenly distributed graphite phase can ensure the low density and neutron moderation of the composite material. Meanwhile, the density and the processing performance of the composite material can be regulated and controlled by regulating the sintering temperature and the heat preservation time, so that the performance requirements of different application scenes are realized, and the method has the advantages of stable process and low cost.
The carbon-based composite material separated by the continuous silicon carbide ceramic has the excellent performances of light weight, high strength, oxidation resistance and the like, so that the carbon-based composite material can be used as an air-cooled micro-stack structural material taking air as a cooling medium.
Drawings
FIG. 1 is an XRD pattern of a carbon-based composite of silicon carbide coated mesophase carbon microsphere composite powder and continuous silicon carbide ceramic separation prepared in example 1 of the present invention.
FIG. 2 is a photomicrograph of a carbon-based composite material (b) of silicon carbide coated mesophase carbon microsphere composite powder (a) and continuous silicon carbide ceramic separation prepared in example 1 of the present invention.
FIG. 3 is an oxidation-weight loss curve of a continuous silicon carbide ceramic-partitioned carbon-based composite prepared in example 1 of the present invention.
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present invention and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that the embodiments of the invention described herein may be implemented in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the attached drawing figures:
the silicon carbide reinforced carbon-based composite material and the preparation process thereof are completed through two steps of combustion synthesis and spark plasma sintering: firstly, the mixed silica powder, the mesocarbon microbeads and the polytetrafluoroethylene reaction promoter powder are filled into a stainless steel die, and the mixed powder is pressed into a reactant sample at a pressure of 30 MPa. Placing a reactant sample into the bottom of a graphite crucible of a combustion synthesis furnace chamber, and covering the reactant sample with composite ignition agent powder; and (3) vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the pressure of 0.5-3 MPa, electrifying the graphite paper tape for 40 seconds to ignite the ignition agent blank, performing a combustion reaction, and grinding the reacted block sample to obtain the composite powder of the silicon carbide coated mesophase carbon microsphere. Fully mixing the composite powder with a composite sintering additive, filling the mixture into a graphite mold, prepressing and forming the mixture under the pressure of 30MPa, and maintaining the pressure for 3-10 minutes; and placing the graphite mold with the pre-pressed sample at the center positions of the upper graphite cushion block and the lower graphite cushion block, and starting a pressure loading system to apply axial pressure of 30-70 MPa to the graphite cushion blocks at the two ends through a pressurizing device. Closing the furnace chamber, and vacuumizing the whole furnace chamber through a vacuum system to form a vacuum chamber with the air pressure less than 5 Pa. Sintering is carried out under the vacuum or inert gas protection condition, and the temperature in the sintering process is measured by an infrared temperature measuring device. During sintering, the power supply system realizes the temperature rise in the furnace chamber through the heating element by current, and then transfers heat to the raw materials to realize reaction sintering. And after the heat preservation process is finished, cooling to room temperature along with the furnace.
Example 1
Silicon powder and mesophase carbon microspheres with a molar ratio of 1:4 are weighed as raw material powder, polytetrafluoroethylene is weighed according to a mass ratio of reaction accelerator to raw material=1:10, mixed powder consisting of the raw material powder and the reaction accelerator is put into an agate mixing tank, and grinding balls are put into the agate mixing tank according to a mass ratio of agate grinding balls to mixed powder=5:1; taking absolute ethyl alcohol according to the mass ratio of absolute ethyl alcohol to mixed powder=1:1, and adding the absolute ethyl alcohol into an agate mixing tank; the agate mixing tank is fixed on a planetary mixer, ball milling is carried out for 2 hours at the rotating speed of 200 revolutions per minute, and the reaction raw material powder is obtained after drying. Placing a reactant sample into the bottom of a graphite crucible of a combustion synthesis furnace chamber, and covering the reactant sample with composite ignition agent powder; and (3) vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the pressure of 2MPa, electrifying the graphite paper tape for 40 seconds to ignite the igniting agent blank, performing a combustion reaction, and grinding the reacted block sample to obtain the composite powder of the silicon carbide coated mesophase carbon microsphere. Taking the composite powder as sintering raw material powder, weighing aluminum oxide and yttrium oxide with the molar ratio of 5:3 as sintering aids, wherein the mass ratio of the sintering aids to the sintering raw material powder is 1:20. Placing the weighed mixed powder consisting of the sintering raw material powder and the sintering auxiliary agent into an agate mixing tank, and placing the agate grinding balls into the agate mixing tank according to the mass ratio of agate grinding balls to the mixed powder=5:1; taking absolute ethyl alcohol according to the mass ratio of absolute ethyl alcohol to mixed powder=1:1, and adding the absolute ethyl alcohol into an agate mixing tank; the agate mixing tank is fixed on a planetary mixer, mixed for 2 hours at the rotating speed of 200 revolutions per minute, dried and sieved to obtain the uniformly mixed powder to be burned. The upper and lower pressure heads and the inner wall of the die are respectively pre-padded with a layer of graphite paper, the mixed raw material powder is put into the graphite die, and the die is pre-pressed and molded under the pressure of 50MPa, and the pressure is maintained for 5 minutes; and then placing the graphite mould into a discharge plasma sintering device, and vacuumizing the furnace chamber to form a vacuum chamber with the pressure in the chamber being less than 5 Pa. An axial pressure of 50MPa is applied to the graphite mold by a loading system. At the beginning of the sintering process, the sample is activated for 60 seconds by using pulse current; in the sintering heating process, the temperature is raised to 1000 ℃ from room temperature at a heating rate of 200-300 ℃/min, the temperature is raised to 1400 ℃ from 1000 ℃ at a heating rate of 150-200 ℃/min, and the temperature is raised to 1700 ℃ from 1400 ℃ at a heating rate of 100-150 ℃/min for 5 min in the first stage. And then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic skeleton reinforced isotropic carbon-based composite material.
The silicon carbide coated intermediate phase carbon microsphere composite powder prepared in the embodiment and the carbon-based composite material separated by the continuous silicon carbide ceramic are subjected to phase analysis by using an X-ray diffractometer (XRD), the XRD pattern is referred to in figure 1, and as can be seen from the figure, the obtained composite powder and the sintered composite material mainly consist of silicon carbide and graphite phases, the composite material contains a small amount of eutectic phase formed by the composite sintering aid, and no silicon phase or other impurity phase exists, so that the silicon and the intermediate phase carbon microsphere can be fully reacted by combustion synthesis, and a silicon carbide ceramic coating layer is generated; spark plasma sintering may promote densification of the composite material through a liquid phase formed by the composite sintering aid. The silicon carbide coated mesophase carbon microsphere composite powder prepared in the embodiment and the carbon-based composite material separated by the continuous silicon carbide ceramic are characterized by using a Field Emission Scanning Electron Microscope (FESEM), the microstructure of the composite material can be referred to as figure 2, and the coated powder of the silicon carbide coated on the surface core-shell structure of the mesophase carbon microsphere can be obviously observed from the figure (a) of figure 2; from fig. 2 (b), it can be observed that a continuous silicon carbide ceramic reinforcing phase is formed in the composite material, separating the mesophase carbon microbeads from each other. The density of the sample was measured by the Archimedes drainage method and found to be 2.62g/cm 3 The relative density is 98.26%, and the apparent porosity is 1.18%; the test result of the three-point bending strength shows that the bending strength of the sample is 238MPa; the test results of oxidation resistance in medium and high temperature air environment show that the mass loss of the sample after oxidation in 900 ℃ air for 1 hour is 3.4%.
Example 2
The process of this example is the same as that of example 1, except that some process parameters are changed: the molar ratio of the silicon powder to the mesophase carbon microsphere is 1:3, the nitrogen pressure is 3MPa, the axial pressure applied to the sample by the spark plasma sintering device is 70MPa, and the final sintering temperature is 1800 ℃.
The resulting product was characterized for phase and microscopic morphology and the results were similar to example 1. The density of the sample was 2.76g/cm 3 The relative density was 99.27%, the apparent porosity was 0.23%, the flexural strength was 325MPa, and the mass loss by oxidation in air at 900℃for 1 hour was 2.5%.
Example 3
The process of this example is the same as that of example 2, except that some process parameters are changed: the nitrogen pressure is 0.5MPa, the mass ratio of the reaction accelerator to the raw materials is 1:5, and the final sintering temperature is 1500 ℃.
The resulting product was characterized for phase and microscopic morphology and the results were similar to example 1. The density of the sample was 2.65g/cm 3 The relative density was 95.28%, the apparent porosity was 3.85%, the flexural strength was 185MPa, and the mass loss by oxidation in air at 900℃for 1 hour was 4.2%.
Example 4
The process of this example is the same as that of example 1, except that some process parameters are changed: the molar ratio of the silicon powder to the mesophase carbon microsphere is 1:20, the mass ratio of the composite sintering aid to the sintering raw material is 1:10, the axial pressure applied to the sample by the spark plasma sintering device is 30MPa, and the final sintering temperature is 1800 ℃.
The resulting product was characterized for phase and microscopic morphology and the results were similar to example 1. The density of the sample was 2.11g/cm 3 The relative density was 91.13%, the apparent porosity was 6.38%, the flexural strength was 92MPa, and the mass loss by oxidation in air at 900℃for 1 hour was 6.3%.
Example 5
The process of this example is the same as that of example 1, except that some process parameters are changed: the mass ratio of the reaction accelerator to the raw materials is 1:20, the mass ratio of the composite sintering aid to the sintering raw materials is 1:30, and the final sintering temperature is 1600 ℃.
The resulting product was characterized for phase and microscopic morphology and the results were similar to example 1. The density of the sample was 2.49g/cm 3 Opposite toThe density is 93.34%, the apparent porosity is 4.88%, the bending strength is 127MPa, and the mass loss after oxidation in 900 ℃ air for 1 hour is 5.1%.
Example 6
The process of this example is the same as that of example 1, except that some process parameters are changed: the mass ratio of the reaction accelerator to the raw materials is 1:20, the mass ratio of the composite sintering aid to the sintering raw materials is 1:30, and the final sintering temperature is 1800 ℃.
The resulting product was characterized for phase and microscopic morphology and the results were similar to example 1. The density of the sample was 2.49g/cm 3 The relative density was 93.16%, the apparent porosity was 5.15%, the flexural strength was 142MPa, and the mass loss by oxidation in air at 900℃for 1 hour was 4.9%.
In summary, the invention uses the mesocarbon microbeads as matrix phase and silicon carbide as ceramic reinforcing phase, the ceramic reinforcing phase closely surrounds the matrix phase to form isotropic structure composite material with continuous reinforcing phase and separated matrix phase; the preparation method of the invention takes micron-sized silica powder and mesophase carbon microspheres as raw materials, firstly, the raw materials are fully mixed by a planetary ball mill, and then the mixture is pre-pressed and molded and then is burnt for synthesis, thus preparing the composite powder of the silicon carbide coated mesophase carbon microspheres; and then mixing the composite powder with a sintering aid, and performing spark plasma sintering to obtain the carbon-based composite material separated by the continuous silicon carbide ceramic. The nano silicon carbide formed by combustion synthesis can overcome the defect that graphite is difficult to compact, and the silicon carbide ceramic is tightly combined with the mesophase carbon microsphere, so that the high-strength characteristic is provided for the composite material. The continuous silicon carbide ceramic reinforced phase separates and protects the graphite matrix phases from each other, and prevents oxidizing gas from penetrating into the composite material, so that the composite material has good oxidation resistance. The relative density of the composite material is 91.13% -99.27%; the apparent porosity is 0.23 to 6.38 percent; the bending strength is 92-325 MPa, and the mass loss of oxidation in air at 900 ℃ for 1 hour is 2.5-6.3%. The composite material has excellent sintering performance, mechanical performance and oxidation resistance, and can meet the application requirements in the fields of nuclear industry, aerospace and the like.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The carbon-based composite material separated by continuous silicon carbide ceramics is characterized by comprising, by volume, 50% -90% of mesophase carbon microspheres and 10% -50% of silicon carbide ceramics; the mesocarbon microbeads are used as matrix phase, the silicon carbide ceramic is used as reinforcing phase, the reinforcing phase is tightly surrounded around the matrix phase, and the isotropic structure composite material with continuous reinforcing phase and separated matrix phase is formed.
2. The continuous silicon carbide ceramic partitioned carbon-based composite material of claim 1, wherein the carbon-based composite material has a relative density of 91.13% to 99.27%; the apparent porosity is 0.23 to 6.38 percent; the bending strength is 92-325 MPa, and the mass loss of oxidation in air at 900 ℃ for 1 hour is 2.5-6.3%.
3. A method of preparing a continuous silicon carbide ceramic partitioned carbon-based composite material according to claim 1 or 2, comprising: and generating a silicon carbide layer on the surface of the mesophase carbon microsphere in situ by a combustion synthesis method to form coated powder, and sintering the coated powder to form the continuous silicon carbide ceramic separated carbon-based composite material.
4. A method of preparing a continuous silicon carbide ceramic partitioned carbon-based composite material according to claim 3, comprising the steps of:
1) Taking silicon powder and mesophase carbon microspheres as raw materials, fully and uniformly mixing the raw materials with a reaction promoter to obtain reaction raw material powder;
2) Prepressing and forming reaction raw material powder to obtain a prepressing and forming sample, embedding the prepressing and forming sample into a composite ignition agent, performing combustion synthesis under nitrogen atmosphere, and cooling to obtain coated powder of silicon carbide coated mesophase carbon microspheres;
3) Taking the coated powder as a sintering raw material, adding a composite sintering auxiliary agent, and fully and uniformly mixing to obtain powder to be sintered;
4) And (3) carrying out spark plasma sintering on the powder to be sintered at 1500-1800 ℃, carrying out heat preservation treatment and cooling to obtain the carbon-based composite material separated by the continuous silicon carbide ceramic.
5. The method for preparing a carbon-based composite material separated by continuous silicon carbide ceramics according to claim 4, wherein polytetrafluoroethylene is used as a reaction promoter, the particle size of the polytetrafluoroethylene is 5-10 μm, and the purity is more than 99.9%; the mass ratio is 1:1, aluminum powder and aluminum nitride powder are used as a composite ignition agent, wherein the grain diameter range of the aluminum powder is 3-5 mu m, the purity is more than 99.9%, the grain diameter range of the aluminum nitride is 3-5 mu m, and the purity is more than 99.99%; the molar ratio is 5:3, the alumina powder and the yttrium oxide powder are used as composite sintering aids.
6. The method for preparing a carbon-based composite material separated by continuous silicon carbide ceramics according to claim 4, wherein in the step 1), the mole ratio of silicon powder to mesocarbon microbeads is 1 (3-20), the particle size of the mesocarbon microbeads is 8-12 μm, the particle size of the silicon powder is 1-3 μm, and the purity is more than 99.0%; the mass ratio of the reaction accelerator to the raw materials is 1 (5-20).
7. The method for producing a continuous silicon carbide ceramic divided carbon-based composite material according to claim 4, wherein in step 2), the pre-press molding is performed at a pressure of 30MPa for 2 minutes; the pressure of the nitrogen atmosphere is 0.5-3 MPa, and the purity is 99.99%; the current-carrying voltage for combustion synthesis was 20V, the current-carrying current was 60A, and the current-carrying time was 40 seconds.
8. The method for producing a continuous silicon carbide ceramic divided carbon-based composite material according to claim 4, wherein in the step 3), the mass ratio of the composite sintering aid to the sintering material is 1 (10 to 30).
9. The method for producing a continuous silicon carbide ceramic-divided carbon-based composite material according to claim 4, wherein in step 4), spark plasma sintering is performed by applying an axial pressure of 30 to 70MPa to a pre-press-molded sample under vacuum or under a protective atmosphere, and activating the sample with a pulse current for 60 seconds; the temperature system of the heat preservation treatment is divided into three stages, wherein the first stage is to heat up to 1000 ℃ from room temperature at a heating rate of 200-300 ℃/min, the second stage is to heat up to 1400 ℃ from 1000 ℃ at a heating rate of 150-200 ℃/min, and the third stage is to heat up to the final sintering temperature from 1400 ℃ at a heating rate of 100-150 ℃/min; the heat preservation treatment time is 5 minutes.
10. Use of a continuous silicon carbide ceramic partitioned carbon-based composite material according to claim 1 or 2 as a gas cooled micro-stack structural material.
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