CN106747453A - A kind of SiC composite fibres wind the Pintsch process processing method of involucrum - Google Patents
A kind of SiC composite fibres wind the Pintsch process processing method of involucrum Download PDFInfo
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- CN106747453A CN106747453A CN201611115400.2A CN201611115400A CN106747453A CN 106747453 A CN106747453 A CN 106747453A CN 201611115400 A CN201611115400 A CN 201611115400A CN 106747453 A CN106747453 A CN 106747453A
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Abstract
The present invention provides the Pintsch process processing method that a kind of SiC composite fibres wind involucrum, and it comprises the following steps：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, is evacuated to below 20Pa；Step 2：Continuing to be passed through argon gas makes body of heater reach 0.1~0.105MPa of pressure-fired, and the state for keep argon gas to be passed through, flow out is started to warm up, and argon gas is passed through and discharge is 1~10L/min, and programming rate is 3~15 DEG C/min；Step 3：When temperature reaches 1000~1600 DEG C, 1~2h is incubated, the involucrum prefabricated component after winding SiC composite fibres occurs cracking reaction；Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample is with stove slow cooling.The present invention devises the process of composite material of silicon carbide cladding tubes cracking, cladding inner after cracking obtains obvious carborundum product, by ceramic phenomenon after follow-up gas-phase permeation significantly, relative density can reach more than 85% to cladding tubes after technique cracking.
Description
Technical field
The invention belongs to nucleus cladding materials manufacturing process area, and in particular to a kind of SiC composite fibres wind involucrum
Pintsch process processing method.
Background technology
At present, all of commercial light-water reactor fuel can is all the alloy with Zr as matrix.This family's material passes through
The reliability of 50 years of researches and application, the performance of nuclear fuel and such fuel can has greatly improved.However,
The service life of zirconium alloy cladding will be influenceed by material corrosion performance, i.e., the oxidation in reactor coolant, especially
The absorption of hydrogen, and, once running into high-temperature steam, the corrosion of zircaloy will be more rapid.Meanwhile, with235U enrichments enter
One step increases, or because the change of other side causes that the amount of fission product in fuel is further raised, this requires research and development
Other materials with more excellent radioresistance injury reinforcing and decay resistance, meanwhile, also require that such material is occurring seriously
Under conditions of accident, the degree of its penalty can be reduced further.Therefore, from the point of view of long-range development trend, exploitation is new
Type cladding materials is imperative.SiC ceramic matrix composite material disclosure satisfy that light-water reactor to greater security, higher performance and higher
The requirement of economy, relative to zirconium alloy cladding, the fuel can advantage with SiC as matrix becomes apparent, specific as follows：
Lower to the absorptivity of thermal neutron (lower than the zirconium cladding of identical wall thickness~25%)；
Be there's almost no in normal course of operation corrosion and hydrogen aggregation, can so greatly improve fuel life-span and
Lift the enrichment of fuel；
Intensity is hardly lost under hot conditions, and corrosion rate is low；
Degradation rate is extremely low during generation major accident：Will not melt down, corrosion rate is low, micro/no hydrogen.
Based on These characteristics, SiC is a kind of cladding materials for having very much an application prospect.Therefore, SiC is carried outf/ SiC is combined
The research of material and its involucrum preparation technology, for the lifting fuel element life-span, improves fuel burn-up and increases reactor and transport
Row economic benefit has great significance.
The content of the invention
It is an object of the invention to provide a kind of Pintsch process handling process method that SiC composite fibres wind involucrum, its
Decomposed by the precursor for after Pintsch process, being solidificated in cladding inner, depositing SiC is obtained between cladding inner fiber
Thing.
Realize the technical scheme of the object of the invention：A kind of SiC composite fibres wind the Pintsch process processing method of involucrum, its
Comprise the following steps：
Step one：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, is evacuated to
Below 20Pa, is filled with argon gas to standard atmospheric pressure, and applying argon gas are vacuumized again, so repeatedly 2~4 times；
Step 2：To continue to be passed through argon gas make body of heater reach 0.1~0.105MPa of pressure-fired, keeps argon gas to be passed through, flows out
State is started to warm up, and argon gas is passed through and discharge is 1~10L/min, and programming rate is 3~15 DEG C/min；
Step 3：When temperature reaches 1000~1600 DEG C, 1~2h is incubated, the involucrum after winding SiC composite fibres is pre-
There is cracking reaction in product；
Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample reaches room temperature with stove slow cooling
When come out of the stove.
A kind of SiC composite fibres as described above wind the Pintsch process processing method of involucrum, and it goes back after step 4
Vapour deposition is carried out to the SiC ceramic matrix composite material cladding tubes after Pintsch process.
A kind of SiC composite fibres as described above wind the Pintsch process processing method of involucrum, described in it in step 4
Vapour deposition also is carried out to the SiC ceramic matrix composite material cladding tubes after Pintsch process afterwards, is comprised the following steps that：
1) heated under the vacuum state first within 20Pa, and be passed through the gaseous mixture of trichloromethyl silane, argon gas, hydrogen
Body, keeps uniform temperature to start deposition；
2) after deposition terminates, SiC ceramic matrix composite material cladding tubes, repeat step 1 are taken out), Multiple depositions are carried out, to obtain difference
The silicon carbide compound cladding tubes of thickness sedimentary.
A kind of SiC composite fibres as described above wind the Pintsch process processing method of involucrum, its described step 1) in, lead to
Enter trichloromethyl silane flow for 100mL/min~5000mL/min, argon flow amount is 2L/min~6L/min, hydrogen flowing quantity is
1L/min~6L/min.
A kind of SiC composite fibres as described above wind the Pintsch process processing method of involucrum, its described step 2) in, gas
1000 DEG C~1200 DEG C of phase depositing temperature, vapor deposition times 6h~60h.
Effect of the invention is that：The present invention uses the means of Pintsch process in silicon carbide compound cladding materials first,
The process of composite material of silicon carbide cladding tubes cracking is devised, optimal parameter is determined by technological experiment, after cracking
Cladding inner obtains obvious carborundum product, and cracking reaction is cmpletely follow-up gas-phase deposition densification
Basis, by ceramic phenomenon after follow-up gas-phase permeation significantly, relative density is reachable for the cladding tubes after the cracking of current technique
To more than 85%.The technique is cladding materials of new generation, and the development and application of silicon carbide fibre enhancing composite involucrum are provided
Technical foundation and guarantee.
Specific embodiment
A kind of Pintsch process of SiC composite fibres winding involucrum of the present invention is processed with reference to specific embodiment
Process is further described.
Embodiment 1
A kind of SiC composite fibres of the present invention wind the Pintsch process processing method of involucrum, and it comprises the following steps：
Step one：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, is evacuated to
Below 20Pa, is filled with argon gas to standard atmospheric pressure, and applying argon gas are vacuumized again, so repeatedly 3 times；
Step 2：Continuing to be passed through argon gas makes body of heater reach pressure-fired 0.1MPa, and the state for keep argon gas to be passed through, flowing out starts
Heat up, argon gas is passed through and discharge is 5L/min, and programming rate is 10 DEG C/min；
Step 3：When temperature reaches 1200 DEG C, 2h is incubated, the involucrum prefabricated component after winding SiC composite fibres occurs
Cracking reaction；
Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample reaches room temperature with stove slow cooling
When come out of the stove.
After the step 4 also to Pintsch process after SiC ceramic matrix composite material cladding tubes carry out vapour deposition, specific steps are such as
Under：
1) heated under the vacuum state first within 20Pa, and be passed through the gaseous mixture of trichloromethyl silane, argon gas, hydrogen
Body, keeps uniform temperature to start deposition；Trichloromethyl silane flow is passed through for 800mL/min, argon flow amount is 4L/min, hydrogen
Flow is 2L/min.1100 DEG C of vapour deposition temperature, vapor deposition times 20h.
2) after deposition terminates, SiC ceramic matrix composite material cladding tubes, repeat step 1 are taken out), 3 depositions are carried out, to obtain difference
The silicon carbide compound cladding tubes of thickness sedimentary.
Embodiment 2
A kind of SiC composite fibres of the present invention wind the Pintsch process processing method of involucrum, and it comprises the following steps：
Step one：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, is evacuated to
Below 20Pa, is filled with argon gas to standard atmospheric pressure, and applying argon gas are vacuumized again, so repeatedly 2 times；
Step 2：Continuing to be passed through argon gas makes body of heater reach pressure-fired 0.105MPa, and the state for keep argon gas to be passed through, flowing out is opened
Begin to heat up, argon gas is passed through and discharge is 1L/min, and programming rate is 3 DEG C/min.
Step 3：When temperature reaches 1000 DEG C, 2h is incubated, the involucrum prefabricated component after winding SiC composite fibres occurs
Cracking reaction；
Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample reaches room temperature with stove slow cooling
When come out of the stove.
Embodiment 3
A kind of SiC composite fibres of the present invention wind the Pintsch process processing method of involucrum, and it comprises the following steps：
Step one：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, is evacuated to
Below 20Pa, is filled with argon gas to standard atmospheric pressure, and applying argon gas are vacuumized again, so repeatedly 4 times；
Step 2：Continuing to be passed through argon gas makes body of heater reach pressure-fired 0.1MPa, and the state for keep argon gas to be passed through, flowing out starts
Heat up, argon gas is passed through and discharge is 10L/min, and programming rate is 15 DEG C/min.
Step 3：When temperature reaches 1600 DEG C, 1h is incubated, the involucrum prefabricated component after winding SiC composite fibres occurs
Cracking reaction；
Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample reaches room temperature with stove slow cooling
When come out of the stove.
After the step 4 also to Pintsch process after SiC ceramic matrix composite material cladding tubes carry out vapour deposition, specific steps are such as
Under：
1) heated under the vacuum state first within 20Pa, and be passed through the gaseous mixture of trichloromethyl silane, argon gas, hydrogen
Body, keeps uniform temperature to start deposition；Trichloromethyl silane flow is passed through for 5000mL/min, argon flow amount is 6L/min, hydrogen
Throughput is 6L/min.1200 DEG C of vapour deposition temperature, vapor deposition times 6h.
2) after deposition terminates, SiC ceramic matrix composite material cladding tubes, repeat step 1 are taken out), 2 depositions are carried out, to obtain difference
The silicon carbide compound cladding tubes of thickness sedimentary.
Embodiment 4
A kind of SiC composite fibres of the present invention wind the Pintsch process processing method of involucrum, and it comprises the following steps：
Step one：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, is evacuated to
Below 20Pa, is filled with argon gas to standard atmospheric pressure, and applying argon gas are vacuumized again, so repeatedly 3 times；
Step 2：Continuing to be passed through argon gas makes body of heater reach pressure-fired 0.1MPa, and the state for keep argon gas to be passed through, flowing out starts
Heat up, argon gas is passed through and discharge is 6L/min, and programming rate is 10 DEG C/min.
Step 3：When temperature reaches 1200 DEG C, 1.5h is incubated, the involucrum prefabricated component after winding SiC composite fibres is sent out
Raw cracking reaction；
Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample reaches room temperature with stove slow cooling
When come out of the stove.
After the step 4 also to Pintsch process after SiC ceramic matrix composite material cladding tubes carry out vapour deposition, specific steps are such as
Under：
1) heated under the vacuum state first within 20Pa, and be passed through the gaseous mixture of trichloromethyl silane, argon gas, hydrogen
Body, keeps uniform temperature to start deposition；Trichloromethyl silane flow is passed through for 100mL/min, argon flow amount is 2L/min, hydrogen
Flow is 1L/min.1000 DEG C of vapour deposition temperature, vapor deposition times 60h.
2) after deposition terminates, SiC ceramic matrix composite material cladding tubes, repeat step 1 are taken out), 4 depositions are carried out, to obtain difference
The silicon carbide compound cladding tubes of thickness sedimentary.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
The various schemes without substantial differences are within the scope of the present invention with present inventive concept.
Claims (5)
1. a kind of SiC composite fibres wind the Pintsch process processing method of involucrum, it is characterised in that：The method includes following step
Suddenly：
Step one：The involucrum prefabricated component that SiC composite fibres are wound is positioned in high temperature sintering furnace, be evacuated to 20Pa with
Under, argon gas to standard atmospheric pressure is filled with, applying argon gas are vacuumized again, so repeatedly 2~4 times；
Step 2：Continuing to be passed through argon gas makes body of heater reach 0.1~0.105MPa of pressure-fired, the state for keeping argon gas to be passed through, flow out
Start to warm up, argon gas is passed through and discharge is 1~10L/min, and programming rate is 3~15 DEG C/min；
Step 3：When temperature reaches 1000~1600 DEG C, 1~2h is incubated, the involucrum prefabricated component after winding SiC composite fibres
Generation cracking reaction；
Step 4：After reaching soaking time, stop heating, continue to be passed through argon gas, sample goes out with stove slow cooling when reaching room temperature
Stove.
2. a kind of SiC composite fibres according to claim 1 wind the Pintsch process processing method of involucrum, and its feature exists
In：After the step 4 also to Pintsch process after SiC ceramic matrix composite material cladding tubes carry out vapour deposition.
3. a kind of SiC composite fibres according to claim 2 wind the Pintsch process processing method of involucrum, and its feature exists
In：It is described after step 4 also to Pintsch process after SiC ceramic matrix composite material cladding tubes carry out vapour deposition, specific steps are such as
Under：
1) heated under the vacuum state first within 20Pa, and be passed through the mixed gas of trichloromethyl silane, argon gas, hydrogen,
Uniform temperature is kept to start deposition；
2) after deposition terminates, SiC ceramic matrix composite material cladding tubes, repeat step 1 are taken out), Multiple depositions are carried out, to obtain different-thickness
The silicon carbide compound cladding tubes of sedimentary.
4. a kind of SiC composite fibres according to claim 3 wind the Pintsch process processing method of involucrum, and its feature exists
In：The step 1) in, trichloromethyl silane flow is passed through for 100mL/min~5000mL/min, argon flow amount is 2L/min
~6L/min, hydrogen flowing quantity is 1L/min~6L/min.
5. a kind of SiC composite fibres according to claim 3 wind the Pintsch process processing method of involucrum, and its feature exists
In：The step 2) in, 1000 DEG C~1200 DEG C of vapour deposition temperature, vapor deposition times 6h~60h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105076A (en) * | 2019-06-12 | 2019-08-09 | 北京理工大学 | A kind of low crash rate SiC ceramic matrix composite material cladding tubes structure of high thermal conductivity and implementation method |
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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 |
-
2016
- 2016-12-07 CN CN201611115400.2A patent/CN106747453B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105076A (en) * | 2019-06-12 | 2019-08-09 | 北京理工大学 | A kind of low crash rate SiC ceramic matrix composite material cladding tubes structure of high thermal conductivity and implementation method |
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