CN111704475B - Chopped silicon carbide fiber reinforced ZrC multilayer cladding material and preparation method thereof - Google Patents
Chopped silicon carbide fiber reinforced ZrC multilayer cladding material and preparation method thereof Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 67
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000000835 fiber Substances 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000005253 cladding Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 17
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008595 infiltration Effects 0.000 claims abstract description 16
- 238000001764 infiltration Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000005011 phenolic resin Substances 0.000 claims abstract description 16
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000006229 carbon black Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 239000011215 ultra-high-temperature ceramic Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000012700 ceramic precursor Substances 0.000 claims abstract description 9
- 238000001746 injection moulding Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- 238000013035 low temperature curing Methods 0.000 claims abstract description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 6
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 6
- 229910000676 Si alloy Inorganic materials 0.000 claims abstract description 5
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical compound [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 73
- 238000000034 method Methods 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 5
- 235000015895 biscuits Nutrition 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000005336 cracking Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000004584 polyacrylic acid Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 102220043159 rs587780996 Human genes 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000000280 densification Methods 0.000 description 7
- 229910001093 Zr alloy Inorganic materials 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
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- 229910045601 alloy Inorganic materials 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 1
- 229910009817 Ti3SiC2 Inorganic materials 0.000 description 1
- 230000002579 anti-swelling effect Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- 230000007246 mechanism Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
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Abstract
The invention relates to the technical field of ZrC ceramic materials, in particular to a chopped silicon carbide fiber reinforced ZrC multilayer cladding material and a preparation method thereof. The preparation method of the chopped silicon carbide fiber reinforced ZrC multilayer coating material comprises the steps of taking aggregate, chopped SiC fiber, carbon black and thermosetting phenolic resin as raw materials, adding a dispersing agent, and carrying out mixing, injection molding, low-temperature curing and high-temperature biscuiting to obtain a porous carbon-containing preform; then, zirconium or zirconium-silicon alloy is used as an infiltrant, and the porous carbon-containing prefabricated body is subjected to high-temperature infiltration sintering to obtain a fiber toughened ultrahigh-temperature ceramic tube; and finally, pulling the plated film in an ethanol solution of the ceramic precursor, and performing high-temperature ceramic conversion to obtain the chopped silicon carbide fiber reinforced ZrC multilayer cladding material. The chopped silicon carbide fiber reinforced ZrC multilayer cladding material has a multilayer structure, high strength and high toughness; the preparation method of the invention realizes the high-efficiency and equal-cost preparation of the cladding material.
Description
Technical Field
The invention relates to the technical field of ZrC ceramic materials, in particular to a chopped silicon carbide fiber reinforced ZrC multilayer cladding material and a preparation method thereof.
Background
As nuclear power technology continues to improve, pressurized water reactor nuclear power plants are moving towards the goal of higher safety and better economy, and as one of the most important components of the reactor, the performance of the fuel assemblies directly affects the safety and economy of the reactor.
Early on, the cladding material was made of Continuous Fiber Ceramic Composite (CFCC), made of aluminum fiber and aluminum matrix, however, it had the disadvantage that fission gases could pass through the compound, and the strength of aluminum after irradiation was greatly reduced, and its application in the field of cladding materials was not suitable. In general, zirconium alloy is mainly used as a cladding material of a pressurized water reactor fuel assembly, but as the internal irradiation time of the zirconium alloy is prolonged, the possibility of breakage of the zirconium alloy is increased, and the zirconium alloy has to be unloaded under the condition that the fuel assembly has quite residual reactivity, so that the cost is higher. At present, the silicon carbide fiber reinforced silicon carbide ceramic matrix composite (SiC) is developing abroadf/SiC) as cladding material, which has a multilayer structure with an intermediate layer of SiCfThe inner surface of the pipe is a compact SiC coating, and the outside of the pipe is a thick compact SiC layer, so that the sealing property and the corrosion resistance of the cladding material are ensured, and the cladding material has better toughness and strength and is an ideal cladding material.
The Ningbo material technology and engineering research institute of Chinese academy of sciences discloses a fiber toughened ceramic matrix composite material with a ternary layered MAX phase interface layer and a preparation method (CN106083117A) thereof, low-oxygen content silicon carbide fibers are obtained through molecular regulation, and high-aluminum (higher than 1 wt%) silicon carbide fibers containing an Al-C chemical bond structure are proposed for the first time to be expected to form a special fiber material for core formation. The development behavior of a ternary laminated MAX phase irradiation damage mechanism and a defect structure is researched, the ternary laminated MAX phase material is proposed and realized for the first time to serve as a SiCf/SiC intermediate layer, and heavy ion irradiation research shows that the novel intermediate layer has good anti-swelling property. Meanwhile, the Ti-Si-C ternary phase diagram is utilized to control the gradient distribution of the phases of the connecting layer, so that the high-strength, low-interface stress, irradiation resistance and corrosion resistance are obtainedReliable connection and TiC/Ti realization3SiC2The full carbide gradient connecting layer is connected with SiC, the problem of interface thermal stress is effectively solved, and the four-point bending strength of the obtained connecting structure is as high as 325 MPa. In addition, a silicon carbide ceramic seamless connection solution is also provided, and a series of 'sacrificial' type ceramic solders are developed to realize the integrated sealing of the silicon carbide ceramic and the composite material.
Northwest industrial university discloses a one-step method for preparing a SiC composite material cladding tube (cn201610429768.x), which comprises the following technical process steps: introducing a layer of one-dimensional SiC nano material on the surface of a mould, weaving a layer of continuous SiC fiber outside the nano material layer to form a SiC fiber preform, and introducing an interface layer into the SiC fiber preform by adopting a chemical vapor deposition method; the interface layer is a pyrolytic carbon PyC layer, a mixed layer of pyrolytic carbon and SiC or Ti3SiC2A layer; and adopting a chemical vapor infiltration process to perform densification treatment on the treated SiC fiber preform, and demolding to obtain the SiC-based cladding tube with a three-layer structure. The process improves the density of the SiC-based cladding tube and the combination between layers, and shortens the preparation period of the SiC-based cladding tube.
However, the preparation processes all adopt silicon carbide fiber preforms, special equipment is needed for weaving, and the process is complex; and the densification is carried out by adopting a chemical vapor infiltration process, the process time is long, the energy consumption is high, the density is not high, the pore defect is easy to form, and the material performance is influenced.
Disclosure of Invention
The invention aims to provide a chopped silicon carbide fiber reinforced ZrC multilayer cladding material which has a multilayer structure, high strength and high toughness; the invention also provides a preparation method of the cladding material, which realizes the high-efficiency and equal-cost preparation of the cladding material and simultaneously ensures the economy and the safety of the cladding material.
The preparation method of the chopped silicon carbide fiber reinforced ZrC multilayer cladding material comprises the following steps:
(1) taking aggregate, chopped SiC fiber, carbon black and thermosetting phenolic resin as raw materials, adding a dispersing agent, and mixing, injection molding, low-temperature curing and high-temperature biscuiting to obtain a porous carbon-containing prefabricated body;
(2) carrying out high-temperature infiltration sintering on the porous carbon-containing prefabricated body by taking zirconium or zirconium-silicon alloy as an infiltration agent to obtain a fiber toughened ultrahigh-temperature ceramic tube;
(3) and taking an ethanol solution of a ceramic precursor as a sol, and carrying out lifting coating and high-temperature ceramic conversion on the fiber-toughened ultrahigh-temperature ceramic tube to obtain the chopped silicon carbide fiber-reinforced ZrC multilayer cladding material.
In the step (1), the raw materials in percentage by mass are:
the addition amount of the dispersing agent is 2-5% of the total mass of the aggregate, the chopped SiC fiber and the carbon black.
Wherein the aggregate is one or two of ZrC and SiC, and the particle size is D50-0.5-5.0 μm;
the length of the short-cut SiC fiber is 1-3 mm;
the thermosetting phenolic resin is one or more of barium phenolic resin, ammonia phenolic resin and boron phenolic resin;
the dispersant is polyacrylic acid.
The mixing process comprises the following steps: the open mill adopts a heating belt for heat preservation, the mixing temperature is 30-90 ℃, and the mixing time is 6-12 h;
the injection molding process comprises the following steps: the injection temperature is 50-120 ℃, the mould is made of graphite and is placed in a vacuum device, and the vacuum degree is 0.1-1 kPa.
The low-temperature curing process comprises the following steps: placing the injection molded biscuit and a mold in a vacuum furnace, wherein the vacuum degree is 0.1-1kPa, heating to 120 ℃ for 10-30min, and preserving heat for 1-2 h; heating to 160 ℃ for 10-60min, and keeping the temperature for 1-2 h; heating to 200 deg.C for 10-60min, and maintaining for 2-4 h.
The high-temperature biscuiting process comprises the following steps: continuing heating and cracking the sample and the mold after low-temperature curing in a vacuum furnace, heating to 350 ℃ within 100-200min, and preserving heat for 2-4 h; heating to 500 deg.C for 60-120min, and maintaining for 2-4 h; raising the temperature to 1400 ℃ at the temperature rise rate of 2-5 ℃/min, and preserving the heat for 1-2 h.
In the step (2), the high-temperature infiltration sintering process comprises the following steps: sintering for 30-60min at the temperature of 1600-2000 ℃ by adopting an embedding method, wherein the dosage of the zirconium or zirconium-silicon alloy is 200% of the mass of the porous carbon-containing prefabricated body.
In the step (3), the ceramic precursor is one or more of polyborosilazane, polycarbosilane and an organic zirconium precursor; in the ethanol solution of the ceramic precursor, the content of the ceramic precursor is 60-90 wt%.
The high-temperature ceramic conversion process comprises the following steps: heating to 120 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h; heating to 350 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h; heating to 500 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h; raising the temperature to 1400 ℃ at the temperature rise rate of 5-10 ℃/min, and preserving the heat for 1-2 h.
And circularly operating the lifting coating process and the high-temperature ceramic conversion process to prepare the sol-gel compact coating until the thickness requirement is met.
The chopped silicon carbide fiber reinforced ZrC multilayer cladding material is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, by designing the raw material composition, curable phenolic resin is introduced into the ceramic powder as a bonding component, so that the molding efficiency of the cladding material is improved, and simple and efficient injection molding is realized;
(2) the invention develops a rapid densification process for a high-strength and high-toughness cladding material, which increases the strength and toughness of the material by introducing silicon carbide chopped fibers and realizes rapid densification of the cladding material by adopting an embedding infiltration process;
(3) the invention develops a rapid preparation method of the compact layer, and the sol-gel method is adopted to prepare the high-performance compact sealing layer, so that the process is simple and the thickness is controllable;
(4) the invention prepares the cladding material with multilayer structure, high strength and high toughness by designing reasonable raw material components and organization structures and reasonable process arrangement, and has simple and easy process, high efficiency and low cost.
Drawings
FIG. 1 is a flow chart of the preparation process of the chopped silicon carbide fiber reinforced ZrC multilayer cladding material.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
(1) Mixing 60 wt% of ZrC (particle size D50 is 2.0 μm), 5 wt% of chopped SiC fibers, 5 wt% of carbon black and 30 wt% of boron phenolic resin serving as raw materials, adding ZrC, chopped SiC fibers and polyacrylic acid accounting for 3% of the total mass of carbon black serving as a dispersing agent, and mixing for 12 hours in an open mill at the mixing temperature of 80 ℃; then placing the mixture in a vacuum device, wherein the vacuum degree is 0.5kPa, and performing injection molding at 100 ℃ by adopting a graphite mold; then placing the injection molded biscuit and the mold in a vacuum furnace, wherein the vacuum degree is 1kPa, heating to 120 ℃ within 30min, preserving heat for 2h, heating to 160 ℃ within 10min, preserving heat for 2h, heating to 200 ℃ within 20min, and preserving heat for 4h to obtain a cured sample; and (3) continuously heating the cured sample and the mold in a vacuum furnace for cracking treatment, heating to 350 ℃ in 100min, preserving heat for 2h, heating to 500 ℃ in 100min, preserving heat for 1h, heating to 1400 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2h to obtain the porous carbon-containing preform.
(2) With Zr90Si10And (3) taking the alloy as an infiltration agent, carrying out high-temperature infiltration sintering on the porous carbon-containing prefabricated body by adopting an embedding method, and carrying out densification sintering at the temperature of 1650 ℃ for 30min to obtain the fiber-toughened ultrahigh-temperature ceramic tube.
(3) Adopting an ethanol solution (80 wt%) of polyborosilazane to carry out drawing coating on the fiber toughened ultrahigh-temperature ceramic tube, then carrying out high-temperature ceramic conversion, heating to 120 ℃ at a heating rate of 5 ℃/min, carrying out heat preservation for 1h, heating to 350 ℃ at a heating rate of 2 ℃/min, carrying out heat preservation for 1h, heating to 500 ℃ at a heating rate of 2 ℃/min, and carrying out heat preservation for 1 h; heating to 1400 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1 h; and repeating the pulling coating and the high-temperature ceramic conversion for 3 times to obtain the chopped silicon carbide fiber reinforced ZrC multilayer cladding material.
Example 2
(1) Using 70 wt% of ZrC (particle size D50 is 2.0 μm), 5 wt% of chopped SiC fibers, 5 wt% of carbon black and 20 wt% of boron phenolic resin as raw materials, adding ZrC, chopped SiC fibers and polyacrylic acid accounting for 2% of the total mass of carbon black as a dispersing agent, and mixing in an open mill at the mixing temperature of 80 ℃ for 10 hours; then placing the mixture in a vacuum device with the vacuum degree of 1kPa, and adopting a graphite mold to perform injection molding at 100 ℃; then placing the injection molded biscuit and the mold in a vacuum furnace, keeping the temperature for 1.5h when the vacuum degree is 1kPa and the temperature rises to 120 ℃ in 30min, keeping the temperature for 2h when the temperature rises to 160 ℃ in 10min, keeping the temperature for 200 ℃ in 20min, and keeping the temperature for 3h to obtain a solidified sample; and (3) continuously heating the cured sample and the mold in a vacuum furnace for cracking treatment, heating to 350 ℃ in 60min, preserving heat for 2h, heating to 500 ℃ in 100min, preserving heat for 1h, heating to 1400 ℃ at the heating rate of 8 ℃/min, and preserving heat for 2h to obtain the porous carbon-containing preform.
(2) And (3) taking Zr powder as an infiltration agent, carrying out high-temperature infiltration sintering on the porous carbon-containing prefabricated body by adopting an embedding method, and carrying out densification sintering at the temperature of 1900 ℃ for 60min to obtain the fiber-toughened ultrahigh-temperature ceramic tube.
(3) Adopting an ethanol solution (80 wt%) of polyborosilazane to carry out drawing coating on the fiber toughened ultrahigh-temperature ceramic tube, then carrying out high-temperature ceramic conversion, heating to 120 ℃ at a heating rate of 5 ℃/min, carrying out heat preservation for 1h, heating to 350 ℃ at a heating rate of 2 ℃/min, carrying out heat preservation for 1h, heating to 500 ℃ at a heating rate of 2 ℃/min, and carrying out heat preservation for 1 h; heating to 1400 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1 h; and repeating the pulling coating and the high-temperature ceramic conversion for 3 times to obtain the chopped silicon carbide fiber reinforced ZrC multilayer cladding material.
Example 3
(1) Using 65 wt% of ZrC (particle size D50 is 2.0 μm), 5 wt% of chopped SiC fibers, 3 wt% of carbon black and 27 wt% of boron phenolic resin as raw materials, adding ZrC, chopped SiC fibers and polyacrylic acid accounting for 5% of the total mass of carbon black as a dispersing agent, and mixing in an open mill at the mixing temperature of 80 ℃ for 10 h; then placing the mixture in a vacuum device, wherein the vacuum degree is 0.7kPa, and performing injection molding at 120 ℃ by adopting a graphite mold; then placing the injection molded biscuit and the mold in a vacuum furnace, wherein the vacuum degree is 1kPa, heating to 120 ℃ within 30min, preserving heat for 2h, heating to 160 ℃ within 10min, preserving heat for 2h, heating to 200 ℃ within 20min, and preserving heat for 4h to obtain a cured sample; and (3) continuously heating the cured sample and the mold in a vacuum furnace for cracking treatment, heating to 350 ℃ in 100min, preserving heat for 2h, heating to 500 ℃ in 100min, preserving heat for 1h, heating to 1400 ℃ at the heating rate of 7 ℃/min, and preserving heat for 2h to obtain the porous carbon-containing preform.
(2) With Zr90Si10And (3) taking the alloy as an infiltration agent, carrying out high-temperature infiltration sintering on the porous carbon-containing prefabricated body by adopting an embedding method, and carrying out densification sintering at 1700 ℃ for 60min to obtain the fiber-toughened ultrahigh-temperature ceramic tube.
(3) Adopting an ethanol solution (80 wt%) of polyborosilazane to carry out drawing coating on the fiber toughened ultrahigh-temperature ceramic tube, then carrying out high-temperature ceramic conversion, heating to 120 ℃ at a heating rate of 5 ℃/min, carrying out heat preservation for 1h, heating to 350 ℃ at a heating rate of 2 ℃/min, carrying out heat preservation for 1h, heating to 500 ℃ at a heating rate of 2 ℃/min, and carrying out heat preservation for 1 h; heating to 1400 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1 h; and repeating the pulling coating and the high-temperature ceramic conversion for 3 times to obtain the chopped silicon carbide fiber reinforced ZrC multilayer cladding material.
The performance criteria for the chopped silicon carbide fiber reinforced ZrC multilayer cladding materials prepared in examples 1-3 are shown in Table 1.
TABLE 1 Performance indices of chopped silicon carbide fiber reinforced ZrC multilayer cladding materials prepared in examples 1-3
| Item | Example 1 | Example 2 | Example 3 |
| Relative density (%) | 99.3 | 98.9 | 98.5 |
| Porosity (%) | 0.3 | 0.3 | 0.5 |
| Bending strength (MPa) | 467 | 573 | 657 |
Claims (9)
1. A preparation method of a chopped silicon carbide fiber reinforced ZrC multilayer cladding material is characterized by comprising the following steps: the method comprises the following steps:
(1) taking aggregate, chopped SiC fiber, carbon black and thermosetting phenolic resin as raw materials, adding a dispersing agent, and mixing, injection molding, low-temperature curing and high-temperature biscuiting to obtain a porous carbon-containing prefabricated body;
(2) carrying out high-temperature infiltration sintering on the porous carbon-containing prefabricated body by taking zirconium or zirconium-silicon alloy as an infiltration agent to obtain a fiber toughened ultrahigh-temperature ceramic tube;
(3) taking an ethanol solution of a ceramic precursor as a sol, and carrying out lifting coating and high-temperature ceramic conversion on the fiber-toughened ultrahigh-temperature ceramic tube to obtain a chopped silicon carbide fiber-reinforced ZrC multilayer cladding material;
in the step (1), the raw materials in percentage by mass are:
60 to 70 percent of aggregate
Chopped SiC fibre 5%
3 to 5 percent of carbon black
20-30% of thermosetting phenolic resin;
the addition amount of the dispersant is 2-5% of the total mass of the aggregate, the chopped SiC fiber and the carbon black;
the aggregate is ZrC, and the particle size is D50= 0.5-5.0 μm;
in the step (3), the ceramic precursor is polyborosilazane.
2. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (1), the length of the chopped SiC fibers is 1-3 mm;
the thermosetting phenolic resin is one or more of barium phenolic resin, ammonia phenolic resin and boron phenolic resin;
the dispersant is polyacrylic acid.
3. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (1), the mixing process comprises the following steps: the open mill adopts a heating belt for heat preservation, the mixing temperature is 30-90 ℃, and the mixing time is 6-12 h;
the injection molding process comprises the following steps: the injection temperature is 50-120 ℃, the mould is made of graphite and is placed in a vacuum device, and the vacuum degree is 0.1-1 kPa.
4. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (1), the low-temperature curing process comprises the following steps: placing the injection molded biscuit and a mold in a vacuum furnace, wherein the vacuum degree is 0.1-1kPa, heating to 120 ℃ for 10-30min, and preserving heat for 1-2 h; heating to 160 ℃ for 10-60min, and keeping the temperature for 2 h; heating to 200 deg.C for 10-60min, and maintaining for 2-4 h;
the high-temperature biscuiting process comprises the following steps: continuing heating and cracking the sample and the mold after low-temperature curing in a vacuum furnace, heating to 350 ℃ within 100-200min, and preserving heat for 2-4 h; heating to 500 deg.C for 60-120min, and maintaining for 2-4 h; heating to 1400 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h.
5. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (2), the high-temperature infiltration sintering process comprises the following steps: sintering at 1600-1800 deg.c for 30-60min by embedding process.
6. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (2), the amount of the zirconium or zirconium-silicon alloy is 200% of the mass of the porous carbon-containing preform.
7. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (3), the content of the ceramic precursor in the ethanol solution of the ceramic precursor is 60-90 wt%.
8. The method for preparing a chopped silicon carbide fiber reinforced ZrC multilayer cladding material as claimed in claim 1, wherein: in the step (3), the high-temperature ceramic conversion process comprises the following steps: heating to 120 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h; heating to 350 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h; heating to 500 ℃ at the heating rate of 2-5 ℃/min, and keeping the temperature for 1-2 h; raising the temperature to 1400 ℃ at the temperature rise rate of 5-10 ℃/min, and preserving the heat for 1-2 h.
9. A short cut silicon carbide fiber reinforced ZrC multilayer cladding material is characterized in that: prepared by the preparation method of any one of claims 1 to 8.
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