CN106747453B - High-temperature cracking treatment method for SiC composite fiber winding cladding - Google Patents
High-temperature cracking treatment method for SiC composite fiber winding cladding Download PDFInfo
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- 238000005253 cladding Methods 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 239000000835 fiber Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005336 cracking Methods 0.000 title claims abstract description 24
- 238000004804 winding Methods 0.000 title claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 100
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 57
- 229910052786 argon Inorganic materials 0.000 claims abstract description 50
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims description 20
- 238000007740 vapor deposition Methods 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 238000000197 pyrolysis Methods 0.000 claims description 11
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- 239000000446 fuel Substances 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 229910001093 Zr alloy Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
- G21C3/02—Fuel elements
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Abstract
The invention provides a high-temperature cracking treatment method for SiC composite fiber wound cladding, which comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, and vacuumizing to below 20 Pa; step two: continuously introducing argon to enable the furnace body to reach a micro positive pressure of 0.1-0.105 MPa, keeping the state of introducing and flowing out of argon, and starting to heat, wherein the introducing and flowing-out amount of argon is 1-10L/min, and the heating speed is 3-15 ℃/min; step three: when the temperature reaches 1000-1600 ℃, preserving the heat for 1-2 h to enable the cladding prefabricated member wound by the SiC composite fibers to have a cracking reaction; step four: and stopping heating after the heat preservation time is reached, continuously introducing argon, and slowly cooling the sample along with the furnace. The invention designs a technological method for cracking the silicon carbide composite material cladding tube, an obvious silicon carbide product is obtained in the cracked cladding tube, the cladding tube subjected to the technological cracking has an obvious ceramic phenomenon after subsequent gas phase permeation, and the relative density can reach more than 85%.
Description
Technical Field
The invention belongs to the field of novel nuclear cladding material manufacturing processes, and particularly relates to a high-temperature cracking treatment method for SiC composite fiber wound cladding.
Background
Currently, all commercial light water reactor fuel cladding are Zr-based alloys. After more than 50 years of research and application, the performance of the nuclear fuel and the reliability of the fuel cladding are greatly improved. However, the service life of the zirconium alloy cladding is affected by the corrosive properties of the material, i.e., oxidation in the reactor coolant, particularly hydrogen absorption, and the zirconium alloy corrodes more rapidly upon exposure to high temperature steam. At the same time, with235Further increase in U enrichment, or further increase in the amount of fission products in the fuel due to other changes, whichIt is required to develop other materials having more excellent radiation damage resistance and corrosion resistance, and also to further reduce the deterioration degree of such materials under severe accident conditions. Therefore, in view of the long-term development trend, the development of new cladding materials is imperative. The SiC composite material can meet the requirements of a light water reactor on higher safety, higher performance and higher economy, and compared with zirconium alloy cladding, the SiC-based fuel cladding has more obvious advantages, specifically as follows:
lower absorption of thermal neutrons (25% lower than a zirconium cladding of the same wall thickness);
corrosion and hydrogen accumulation hardly exist in the normal operation process, so that the service life of the fuel can be greatly prolonged, and the enrichment degree of the fuel can be improved;
almost no strength loss under high temperature condition and low corrosion rate;
the degradation rate is extremely low when major accidents occur: no melting damage, low corrosion rate and trace/no hydrogen.
Based on the characteristics, SiC is a cladding material with great application prospect. Thus, SiC was developedfThe research on the preparation process of the/SiC composite material and the cladding thereof has important significance for prolonging the service life of fuel elements, improving fuel consumption and increasing the economic benefits of reactor operation.
Disclosure of Invention
The invention aims to provide a high-temperature cracking treatment process method for SiC composite fiber wound cladding.
The technical scheme for realizing the purpose of the invention is as follows: a pyrolysis treatment method for SiC composite fiber winding cladding comprises the following steps:
the method comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, vacuumizing to below 20Pa, filling argon to standard atmospheric pressure, vacuumizing again, filling argon, and repeating the steps for 2-4 times;
step two: continuously introducing argon to enable the furnace body to reach a micro positive pressure of 0.1-0.105 MPa, keeping the state of introducing and flowing out of argon, and starting to heat, wherein the introducing and flowing-out amount of argon is 1-10L/min, and the heating speed is 3-15 ℃/min;
step three: when the temperature reaches 1000-1600 ℃, preserving the heat for 1-2 h to enable the cladding prefabricated member wound by the SiC composite fibers to have a cracking reaction;
step four: and stopping heating after the heat preservation time is reached, continuously introducing argon, slowly cooling the sample along with the furnace, and discharging the sample from the furnace when the temperature reaches the room temperature.
The pyrolysis treatment method for the SiC composite fiber winding cladding is characterized in that after the fourth step, the SiC composite cladding tube after pyrolysis is also subjected to vapor deposition.
According to the pyrolysis treatment method for the SiC composite fiber wound cladding, the SiC composite material cladding tube subjected to pyrolysis is subjected to vapor deposition after the fourth step, and the method comprises the following specific steps:
1) firstly, heating under the vacuum condition within 20Pa, introducing mixed gas of trichloromethylsilane, argon and hydrogen, and keeping a certain temperature to start deposition;
2) and after the deposition is finished, taking out the SiC composite cladding tube, and repeating the step 1) for multiple depositions to obtain the silicon carbide composite cladding tube with different thickness deposition layers.
According to the high-temperature cracking treatment method for the SiC composite fiber wound cladding, in the step 1), trichloromethylsilane is introduced at a flow rate of 100-5000 mL/min, argon flow rate is 2-6L/min, and hydrogen flow rate is 1-6L/min.
According to the high-temperature cracking treatment method for the SiC composite fiber wound cladding, in the step 2), the vapor deposition temperature is 1000-1200 ℃, and the vapor deposition time is 6-60 h.
The invention has the following effects: the invention adopts a high-temperature cracking means in the silicon carbide composite cladding material for the first time, designs a technological method for cracking the silicon carbide composite cladding tube, determines the optimal parameters through technological experiments, obtains obvious silicon carbide products in the cracked cladding tube, and completely and fully carries out the cracking reaction to be the basis of the densification of the subsequent vapor deposition process, and the cladding tube cracked by the prior art has obvious ceramic phenomenon after the subsequent vapor permeation, and the relative density can reach more than 85 percent. The process provides a technical basis and guarantee for the development and application of a new generation of cladding material and the cladding of the silicon carbide fiber reinforced composite material.
Detailed Description
The pyrolysis treatment process of the SiC composite fiber wound cladding of the invention is further described with reference to the specific embodiment.
Example 1
The invention relates to a high-temperature cracking treatment method for SiC composite fiber wound cladding, which comprises the following steps:
the method comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, vacuumizing to below 20Pa, filling argon to standard atmospheric pressure, vacuumizing again, filling argon, and repeating the steps for 3 times;
step two: continuously introducing argon to enable the furnace body to reach a micro positive pressure of 0.1MPa, keeping the state of introducing and flowing out of the argon, and starting to heat, wherein the introducing and flowing-out amount of the argon is 5L/min, and the heating speed is 10 ℃/min;
step three: when the temperature reaches 1200 ℃, preserving the heat for 2 hours to ensure that the cladding prefabricated member wound by the SiC composite fibers has a cracking reaction;
step four: and stopping heating after the heat preservation time is reached, continuously introducing argon, slowly cooling the sample along with the furnace, and discharging the sample from the furnace when the temperature reaches the room temperature.
And after the fourth step, carrying out vapor deposition on the SiC composite cladding tube subjected to pyrolysis, and specifically comprising the following steps of:
1) firstly, heating under the vacuum condition within 20Pa, introducing mixed gas of trichloromethylsilane, argon and hydrogen, and keeping a certain temperature to start deposition; the flow rate of trichloromethylsilane introduced is 800mL/min, the flow rate of argon is 4L/min, and the flow rate of hydrogen is 2L/min. The vapor deposition temperature is 1100 ℃, and the vapor deposition time is 20 h.
2) And after the deposition is finished, taking out the SiC composite cladding tube, and repeating the step 1) for 3 times of deposition to obtain the silicon carbide composite cladding tube with the deposition layers of different thicknesses.
Example 2
The invention relates to a high-temperature cracking treatment method for SiC composite fiber wound cladding, which comprises the following steps:
the method comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, vacuumizing to below 20Pa, filling argon to standard atmospheric pressure, vacuumizing again, filling argon, and repeating the steps for 2 times;
step two: and continuously introducing argon to ensure that the furnace body reaches a micro positive pressure of 0.105MPa, keeping the state of introducing and flowing out of the argon, and starting to heat, wherein the introducing and flowing-out amount of the argon is 1L/min, and the heating speed is 3 ℃/min.
Step three: when the temperature reaches 1000 ℃, preserving the heat for 2 hours to ensure that the cladding prefabricated member wound by the SiC composite fibers has a cracking reaction;
step four: and stopping heating after the heat preservation time is reached, continuously introducing argon, slowly cooling the sample along with the furnace, and discharging the sample from the furnace when the temperature reaches the room temperature.
Example 3
The invention relates to a high-temperature cracking treatment method for SiC composite fiber wound cladding, which comprises the following steps:
the method comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, vacuumizing to below 20Pa, filling argon to standard atmospheric pressure, vacuumizing again, filling argon, and repeating the steps for 4 times;
step two: and continuously introducing argon to ensure that the furnace body reaches a micro positive pressure of 0.1MPa, keeping the state of introducing and flowing out of the argon, and starting to heat, wherein the introducing and flowing-out amount of the argon is 10L/min, and the heating speed is 15 ℃/min.
Step three: when the temperature reaches 1600 ℃, preserving the heat for 1h to ensure that the cladding prefabricated member wound by the SiC composite fibers has a cracking reaction;
step four: and stopping heating after the heat preservation time is reached, continuously introducing argon, slowly cooling the sample along with the furnace, and discharging the sample from the furnace when the temperature reaches the room temperature.
And after the fourth step, carrying out vapor deposition on the SiC composite cladding tube subjected to pyrolysis, and specifically comprising the following steps of:
1) firstly, heating under the vacuum condition within 20Pa, introducing mixed gas of trichloromethylsilane, argon and hydrogen, and keeping a certain temperature to start deposition; the flow rate of trichloromethylsilane introduced is 5000mL/min, the flow rate of argon is 6L/min, and the flow rate of hydrogen is 6L/min. The vapor deposition temperature is 1200 ℃, and the vapor deposition time is 6 h.
2) And after the deposition is finished, taking out the SiC composite cladding tube, and repeating the step 1) for 2 times of deposition to obtain the silicon carbide composite cladding tube with the deposition layers of different thicknesses.
Example 4
The invention relates to a high-temperature cracking treatment method for SiC composite fiber wound cladding, which comprises the following steps:
the method comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, vacuumizing to below 20Pa, filling argon to standard atmospheric pressure, vacuumizing again, filling argon, and repeating the steps for 3 times;
step two: and continuously introducing argon to ensure that the furnace body reaches a micro positive pressure of 0.1MPa, keeping the state of introducing and flowing out of the argon, and starting to heat, wherein the introducing and flowing-out amount of the argon is 6L/min, and the heating speed is 10 ℃/min.
Step three: when the temperature reaches 1200 ℃, preserving the heat for 1.5h to enable the cladding prefabricated member wound by the SiC composite fibers to have a cracking reaction;
step four: and stopping heating after the heat preservation time is reached, continuously introducing argon, slowly cooling the sample along with the furnace, and discharging the sample from the furnace when the temperature reaches the room temperature.
And after the fourth step, carrying out vapor deposition on the SiC composite cladding tube subjected to pyrolysis, and specifically comprising the following steps of:
1) firstly, heating under the vacuum condition within 20Pa, introducing mixed gas of trichloromethylsilane, argon and hydrogen, and keeping a certain temperature to start deposition; the flow rate of trichloromethylsilane introduced is 100mL/min, the flow rate of argon is 2L/min, and the flow rate of hydrogen is 1L/min. The vapor deposition temperature is 1000 ℃, and the vapor deposition time is 60 h.
2) And after the deposition is finished, taking out the SiC composite cladding tube, and repeating the step 1) for 4 times of deposition to obtain the silicon carbide composite cladding tube with the deposition layers of different thicknesses.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned examples, and various schemes which are not substantially different from the concept of the present invention are within the protection scope of the present invention.
Claims (2)
1. A high-temperature cracking treatment method for SiC composite fiber winding cladding is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: placing a cladding prefabricated part formed by winding SiC composite fibers in a high-temperature sintering furnace, vacuumizing to below 20Pa, filling argon to standard atmospheric pressure, vacuumizing again, filling argon, and repeating the steps for 2-4 times;
step two: continuously introducing argon to enable the furnace body to reach a micro positive pressure of 0.1-0.105 MPa, keeping the state of introducing and flowing out of argon, and starting to heat, wherein the introducing and flowing-out amount of argon is 1-10L/min, and the heating speed is 3-15 ℃/min;
step three: when the temperature reaches 1000-1600 ℃, preserving the heat for 1-2 h to enable the cladding prefabricated member wound by the SiC composite fibers to have a cracking reaction;
step four: stopping heating after the heat preservation time is reached, continuously introducing argon, slowly cooling the sample along with the furnace, and discharging the sample from the furnace when the temperature reaches the room temperature;
and after the fourth step, carrying out vapor deposition on the SiC composite cladding tube subjected to pyrolysis, and specifically comprising the following steps of:
1) firstly, heating under the vacuum condition within 20Pa, introducing mixed gas of trichloromethylsilane, argon and hydrogen, and keeping a certain temperature to start deposition;
2) after deposition is finished, taking out the SiC composite material cladding tube, repeating the step 1), and performing deposition for multiple times to obtain silicon carbide composite cladding tubes with deposition layers of different thicknesses; the vapor deposition temperature is 1000-1200 ℃, and the vapor deposition time is 6-60 h.
2. The method of claim 1, wherein the pyrolysis treatment of the SiC composite fiber wound cladding comprises: in the step 1), the flow rate of trichloromethylsilane is 100mL/min to 5000mL/min, the flow rate of argon is 2L/min to 6L/min, and the flow rate of hydrogen is 1L/min to 6L/min.
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| CN103818056A (en) * | 2013-12-27 | 2014-05-28 | 西北工业大学 | Multilayer structure of SiC/SiC (silicon carbide) composite cladding tube and preparation method thereof |
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| US5391428A (en) * | 1992-06-12 | 1995-02-21 | Minnesota Mining And Manufacturing Company | Monolithic ceramic/fiber reinforced ceramic composite |
| CN101019193A (en) * | 2004-06-07 | 2007-08-15 | 西屋电气有限责任公司 | Multi-layered ceramic tube for fuel containment barrier and other applications in nuclear and fossil power plants |
| CN106342085B (en) * | 2006-07-03 | 2011-02-16 | 中国科学院上海硅酸盐研究所 | A kind of processing method of improving silicon carbide fibre serviceability temperature and performance |
| CN102203879A (en) * | 2008-09-18 | 2011-09-28 | 原子能与可替代能源委员会 | Nuclear fuel sheath with high heat conductivity and method for making same |
| CN103818056A (en) * | 2013-12-27 | 2014-05-28 | 西北工业大学 | Multilayer structure of SiC/SiC (silicon carbide) composite cladding tube and preparation method thereof |
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