CN113012834A - Preparation method of uranium nitride composite uranium trisilicon two-fuel pellet - Google Patents
Preparation method of uranium nitride composite uranium trisilicon two-fuel pellet Download PDFInfo
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- CN113012834A CN113012834A CN201911335506.7A CN201911335506A CN113012834A CN 113012834 A CN113012834 A CN 113012834A CN 201911335506 A CN201911335506 A CN 201911335506A CN 113012834 A CN113012834 A CN 113012834A
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C21/00—Apparatus or processes specially adapted to the manufacture of reactors or parts thereof
- G21C21/02—Manufacture of fuel elements or breeder elements contained in non-active casings
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C21/00—Apparatus or processes specially adapted to the manufacture of reactors or parts thereof
- G21C21/02—Manufacture of fuel elements or breeder elements contained in non-active casings
- G21C21/16—Manufacture of fuel elements or breeder elements contained in non-active casings by casting or dipping techniques
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention belongs to the technical field of preparation of uranium nitride composite fuel pellets, and particularly relates to a preparation method of a uranium nitride composite uranium three-silicon two-fuel pellet. U is prepared by vacuum induction melting of metallic uranium and elemental silicon3Si2Crushing and ball-milling the ingot to obtain U3Si2Powder; preparing metal uranium powder from the metal uranium through cyclic hydrogenation and dehydrogenation, and nitriding to obtain a uranium nitrogen compound; placing the uranium nitrogen compound in a graphite die for prepressing, performing high-temperature denitrification in a tungsten-molybdenum sintering furnace together with the die and the uranium nitrogen compound, obtaining a massive UN material after denitrification, and preparing UN powder which can stably exist at room temperature after crushing and ball milling; mixing UN powder with 10-80 wt% of U3Si2Powder is subjected to dry three-dimensional mixing or wet ball milling mixing by taking ethanol as a medium to obtain UN-U3Si2Mixing the powders, and sintering under pressureless or hot pressing to obtain UN-U3Si2A composite fuel pellet. The pellet has higher uranium density, higher heat conductivity coefficient and certain steam oxidation resistance, and the integral capability of a system for bearing serious accident conditions is enhanced.
Description
Technical Field
The invention belongs to the technical field of preparation of uranium nitride composite fuel pellets, and particularly relates to a preparation method of a uranium nitride composite uranium three-silicon two-fuel pellet.
Background
The preparation method of the current widely used foreign technology is to mix U3Si2Mixing with UN, and liquid phase sintering or spark plasma sintering to obtain UN-U3Si2The preparation process of the composite fuel is unclear, and domestic research on the composite fuel is not reported yet.
Disclosure of Invention
The invention aims to provide a preparation method of uranium nitride composite uranium trisilicon two-fuel pellets, and prepared UN-U3Si2Composite fuel and conventional UO2Compared with the fuel pellet, the fuel pellet has higher uranium density, higher heat conductivity coefficient and certain steam oxidation resistance, and the overall capability of the system for bearing serious accident conditions is enhanced.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing uranium nitride composite uranium trisilicon two fuel pellets,
(1) u is prepared by vacuum induction melting of metallic uranium and elemental silicon3Si2Crushing and ball-milling the ingot to obtain U3Si2Powder;
(2) preparing metal uranium powder from the metal uranium through cyclic hydrogenation and dehydrogenation, and nitriding to obtain a uranium nitrogen compound;
(3) placing the uranium nitrogen compound in a graphite die for prepressing, performing high-temperature denitrification in a tungsten-molybdenum sintering furnace together with the die and the uranium nitrogen compound, obtaining a massive UN material after denitrification, and preparing UN powder which can stably exist at room temperature after crushing and ball milling;
(4) mixing UN powder with 10-80 wt% of U3Si2Powder is subjected to dry three-dimensional mixing or wet ball milling mixing by taking ethanol as a medium to obtain UN-U3Si2Mixing the powders, and sintering under pressureless or hot pressing to obtain UN-U3Si2A composite fuel pellet.
And (2) carrying out 1-5 times of cyclic hydrogenation dehydrogenation on the uranium to prepare uranium powder.
In the step (2), the uranium nitride compound UN is obtained by nitridationx，1＜X≤2。
And (3) heating the die and the uranium nitrogen compound together in a tungsten-molybdenum sintering furnace to 1360-1460 ℃ for denitrification.
And (4) if pressureless sintering is adopted, sintering is carried out in a vacuum or inert gas environment at the temperature of 1550-1630 ℃, and the heat preservation time is 4-7 hours.
And (4) if hot-pressing sintering is adopted, placing the material in a hot-pressing die, wherein the hot-pressing pressure is 30-70 MPa, the hot-pressing temperature is 1450-1600 ℃, and the hot-pressing time is 1-2.5 hours.
The beneficial effects obtained by the invention are as follows:
preparing UN powder stably existing in the air and U by optimizing a denitrification process3Si2After being uniformly mixed, the UN-U with higher uranium density, higher heat conductivity coefficient and certain steam oxidation resistance is prepared by pressureless or hot-pressing sintering3Si2A composite fuel pellet.
The new type of accident-resistant fuel that is currently widely accepted internationally includes uranium silicide (U)3Si2、U3Si5) And uranium silicide-uranium nitride (UN-U)3Si2、UN-U3Si5) Composite material with conventional UO2Compared with fuel pellet, the fuel pellet has higher uranium density and higher heat conductivity coefficient, the overall capability of the system for bearing serious accident conditions is enhanced, and both silicides have melting point reduction and multiphase conversion but only U3Si2Providing a higher metal density. The invention uses goldPreparing U by smelting uranium and elemental silicon in two phases3Si2Crushing and ball-milling ingot to obtain U with certain granularity3Si2Powder, which is mixed with UN powder prepared by hydrogenating and dehydrogenating metal uranium and denitrifying nitrogen, and is prepared into UN-U with certain steam oxidation resistance through pressureless sintering or hot-pressing sintering3Si2And (3) compounding the fuel.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The preparation method of the uranium nitride composite uranium trisilicon two fuel pellet comprises the following steps: u is prepared by vacuum induction melting of metallic uranium and elemental silicon3Si2Crushing and ball-milling the ingot to obtain U3Si2Powder; the method comprises the steps of preparing metal uranium powder from metal uranium through 1-5 times of cyclic hydrogenation and dehydrogenation, and nitriding to obtain a uranium nitride compound (UN)xAnd X is more than 1 and less than or equal to 2), placing the uranium nitrogen compound in a graphite mold for prepressing, heating the graphite mold and the uranium nitrogen compound in a tungsten-molybdenum sintering furnace to 1360-1460 ℃ for high-temperature denitrification, obtaining a blocky UN material after denitrification, and preparing the UN powder which can stably exist at room temperature after crushing and ball milling. Mixing UN powder with 10-80 wt% of U3Si2Powder is subjected to dry three-dimensional mixing or wet ball milling mixing by taking ethanol as a medium to obtain UN-U3Si2Mixing the powders, and sintering under pressureless or hot pressing to obtain UN-U3Si2A composite fuel pellet; if pressureless sintering is adopted, sintering is carried out in a vacuum or inert gas environment at the temperature of 1550-1630 ℃, and the heat preservation time is 4-7 hours; and if hot-pressing sintering is adopted, placing the mixture into a hot-pressing die, wherein the hot-pressing pressure is 30-70 MPa, the hot-pressing temperature is 1450-1600 ℃, and the hot-pressing time is 1-2.5 hours.
Examples
Selecting high-purity graphite as a mould for smelting, and coating a layer of refractory oxide slurry coating on the inner wall of the mould in an electrostatic spraying mode, wherein the slurry is formed by ZrO2(wherein 10-20 wt% of Y is added2O3) Composition is carried out;
cleaning an oxide layer on the surface of a refined uranium ingot by using nitric acid, soaking the uranium ingot in alcohol to remove residual dirt on the surface, wiping and drying the uranium ingot, putting the uranium ingot on a high-purity silicon ingot, and putting the uranium ingot into a high-purity graphite crucible, wherein the mass of the silicon ingot accounts for 5-11% of the total mass;
putting the whole mould with the material into a high-frequency induction smelting furnace, charging Ar gas as protective gas, setting the smelting temperature to be 1500-1800 ℃, realizing homogenization of the material by continuously stirring the molten material in the smelting process, and pouring the molten material into the graphite mould with the coating prepared in the step 1 after sufficient degassing;
taking the material out of the graphite die after the material is cooled, primarily breaking the material by using a hammer, grinding the material into powder by using a rod grinder, and sieving the powder to obtain the U with a certain granularity required by the preparation of the composite fuel pellet3Si2Powder;
cleaning an oxide layer of 1kg of metal uranium sheet by nitric acid, soaking the metal uranium sheet in alcohol to remove residual impurities on the surface, wiping the metal uranium sheet dry, placing the metal uranium sheet in a hydrogenation dehydrogenation furnace, introducing hydrogen with the pressure of 0.03-0.07 MPa, hydrogenating the metal uranium sheet at the temperature of 265-280 ℃ for 1-3 hours, vacuumizing and heating to the temperature of 530-570 ℃ for dehydrogenation for 3-5 hours, vacuumizing and cooling to the room temperature, and repeating the hydrogenation dehydrogenation process for 3 times to obtain metal uranium powder with a certain particle size;
continuously introducing nitrogen with the pressure of 0.03-0.07 MPa into the hydrogenation and dehydrogenation furnace, heating the metal uranium powder to 450-500 ℃, nitriding for 6-10 hours, and keeping the positive pressure in the furnace and cooling to room temperature to obtain a uranium nitrogen compound;
loading a uranium nitrogen compound into a phi 40mm steel die in a glove box, wrapping the uranium nitrogen compound with a plastic film after primary prepressing, taking out the glove box, placing the glove box on a four-column hydraulic press, removing the plastic film after 30-50 MPa secondary prepressing, placing the uranium nitrogen compound subjected to secondary prepressing and the die in a tungsten-molybdenum sintering furnace, heating to 1360-1460 ℃ for high-temperature denitrification to obtain a blocky UN material, and crushing and sieving to prepare UN powder capable of stably existing at room temperature;
taking 10-20 gUN powder and 20 wt% of U3Si2Three-dimensionally mixing the powder for 3-6 hours by a dry method to obtain uniformly mixed UN-U3Si2And mixing the powders.
Prepressing a carbide alloy solid die with the diameter of 10.00mm under the pressure of 110-150 MPa to prepare UN-U3Si2And (4) green pressing.
Adopts a tungsten-molybdenum high-temperature sintering furnace with the temperature of 1550-1600 ℃ and the temperature of 10 DEG C-4Sintering under Pa, and keeping the temperature for 5-7 hours to obtain UN-U3Si2A composite fuel pellet.
Claims (6)
1. A preparation method of uranium nitride composite uranium trisilicon two fuel pellets is characterized by comprising the following steps:
(1) u is prepared by vacuum induction melting of metallic uranium and elemental silicon3Si2Crushing and ball-milling the ingot to obtain U3Si2Powder;
(2) preparing metal uranium powder from the metal uranium through cyclic hydrogenation and dehydrogenation, and nitriding to obtain a uranium nitrogen compound;
(3) placing the uranium nitrogen compound in a graphite die for prepressing, performing high-temperature denitrification in a tungsten-molybdenum sintering furnace together with the die and the uranium nitrogen compound, obtaining a massive UN material after denitrification, and preparing UN powder which can stably exist at room temperature after crushing and ball milling;
(4) mixing UN powder with 10-80 wt% of U3Si2Powder is subjected to dry three-dimensional mixing or wet ball milling mixing by taking ethanol as a medium to obtain UN-U3Si2Mixing the powders, and sintering under pressureless or hot pressing to obtain UN-U3Si2A composite fuel pellet.
2. The method for preparing uranium nitride composite uranium trisilicon two fuel pellets according to claim 1, characterized in that: and (2) carrying out 1-5 times of cyclic hydrogenation dehydrogenation on the uranium to prepare uranium powder.
3. The method for preparing uranium nitride composite uranium trisilicon two fuel pellets according to claim 1, characterized in that: in the step (2), the uranium nitride compound UN is obtained by nitridationx，1＜X≤2。
4. The method for preparing uranium nitride composite uranium trisilicon two fuel pellets according to claim 1, characterized in that: and (3) heating the die and the uranium nitrogen compound together in a tungsten-molybdenum sintering furnace to 1360-1460 ℃ for denitrification.
5. The method for preparing uranium nitride composite uranium trisilicon two fuel pellets according to claim 1, characterized in that: and (4) if pressureless sintering is adopted, sintering is carried out in a vacuum or inert gas environment at the temperature of 1550-1630 ℃, and the heat preservation time is 4-7 hours.
6. The method for preparing uranium nitride composite uranium trisilicon two fuel pellets according to claim 1, characterized in that: and (4) if hot-pressing sintering is adopted, placing the material in a hot-pressing die, wherein the hot-pressing pressure is 30-70 MPa, the hot-pressing temperature is 1450-1600 ℃, and the hot-pressing time is 1-2.5 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113816749A (en) * | 2021-10-21 | 2021-12-21 | 中国科学院上海应用物理研究所 | High-density U3Si2Method for producing fuel |
| CN115896495A (en) * | 2022-11-18 | 2023-04-04 | 中核北方核燃料元件有限公司 | Method for rapidly sintering high-uranium-density high-thermal-conductivity composite core block |
| WO2023130356A1 (en) * | 2022-01-07 | 2023-07-13 | 岭澳核电有限公司 | High-uranium-density atf nuclear fuel pellet and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113816749A (en) * | 2021-10-21 | 2021-12-21 | 中国科学院上海应用物理研究所 | High-density U3Si2Method for producing fuel |
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| WO2023130356A1 (en) * | 2022-01-07 | 2023-07-13 | 岭澳核电有限公司 | High-uranium-density atf nuclear fuel pellet and preparation method therefor |
| CN115896495A (en) * | 2022-11-18 | 2023-04-04 | 中核北方核燃料元件有限公司 | Method for rapidly sintering high-uranium-density high-thermal-conductivity composite core block |
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