CN106847353A - Lutetium oxide target piece pellet preparation technology - Google Patents

Lutetium oxide target piece pellet preparation technology Download PDF

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Publication number
CN106847353A
CN106847353A CN201710007383.9A CN201710007383A CN106847353A CN 106847353 A CN106847353 A CN 106847353A CN 201710007383 A CN201710007383 A CN 201710007383A CN 106847353 A CN106847353 A CN 106847353A
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target piece
oxide powder
lutetium oxide
powder
lutetium
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CN106847353B (en
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尹邦跃
屈哲昊
郑新海
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China Institute of Atomic of Energy
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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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/51—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on compounds of actinides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • G21C3/42—Selection of substances for use as reactor fuel
    • G21C3/58—Solid reactor fuel Pellets made of fissile material
    • G21C3/62—Ceramic fuel
    • G21C3/623—Oxide fuels
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
    • 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 nuclear material preparation field.Relatively low to solve overall neptunium useful load present in existing lutetium oxide target piece preparation technology, production cost is higher, the problems such as technique is complex, the invention provides a kind of lutetium oxide target piece pellet preparation technology.The technique is comprised the following steps：(1) lutetium oxide powder is taken with magnesium oxide powder as target piece pellet raw material；(2) take out partial oxidation neptunium powder to mix with magnesium oxide powder, obtain just mixed powder；(3) add remaining lutetium oxide powder and stearic acid to continue to mix, obtain mixed-powder；(4) cold moudling, is made target piece pellet green compact；(5) pressureless sintering, is obtained lutetium oxide target piece pellet.Preparation technology of the invention has technological process simple, low cost and other advantages, and obtained lutetium oxide target piece pellet totality neptunium useful load is high, and neutron utilization rate is high, and possesses higher heat-conductivity, good in in-pile irradiation performance, is easy to chemolysis to extract, it is adaptable to238The large-scale production of Pu fuel.

Description

Lutetium oxide target piece pellet preparation technology
Technical field
The invention belongs to nuclear material preparation field, more particularly to a kind of lutetium oxide target piece pellet preparation technology.
Background technology
238Pu is a kind of important nuclear material in space nuclear field, is the radio isotope electricity needed for carrying out space operation Source and the ideal fuels of thermal source.By taking the U.S. as an example, in the space exploration task in past 60 years, on the spacecraft of its transmitting The 42 radioactive isotope power supply systems carried have selected238Pu is used as fuel.
At present,238The production of Pu is main to be irradiated by reactor237The mode of Np realizes that its principle is：237Np exists There is (n, γ) reaction under neutron irradiation to produce238Np nucleic, generation238There is β decay generations in Np238Pu。
Based on principles above, U.S. Sa Fanna rivers Development of Laboratories NpO2- Al disperse target piece preparation technology (note：Hereafter Middle Np is refered in particular to237Np), its main preparation flow is as follows：First by native oxide neptunium by chemistry such as dissolving, removal of impurities and oxidations Process is made purifying lutetium oxide powder；Then lutetium oxide powder and Al powder are pressed 1:4 volume ratios mix, and annular is pressed into through hot extrusion Target piece core body；Core body assembling is finally made target piece.But the technique is complex, target piece is that annular and lutetium oxide powder are only accounted for The 20% of target piece core body so that overall neptunium useful load is relatively low, causes238Pu yield is relatively low, and production cost is higher.
The U.S. stopped production in 1988238Pu, and big rule were lost after the K reactor shut-downs of Sa Fanna rivers in 1996 Mould238The production capacity of Pu.2013, USDOE restarted238The production of Pu, has still selected more ripe at present NpO2- Al disperse target piece preparation technologies, and the development of the new technology such as ceramic target, liquid target related to neptunium target piece is also being entered Among row, have no that ripe technique is published so far.
The content of the invention
Relatively low to solve overall neptunium useful load present in existing lutetium oxide target piece preparation technology, production cost is higher, work The problems such as skill is complex, the invention provides a kind of lutetium oxide target piece pellet preparation technology.The technique is comprised the following steps：
(1) lutetium oxide powder is taken as needed with magnesium oxide powder as target piece pellet raw material, wherein, magnesium oxide powder Quality account for the 1-10% of the two gross mass；
(2) in the lutetium oxide powder, taking-up accounts for the lutetium oxide powder of 0.5-4 times of the magnesium oxide powder quality, will The lutetium oxide powder of taking-up mixes more than 4h with the magnesium oxide powder in three-dimensional motion mixer, obtains just mixed powder；
(3) remaining lutetium oxide powder and stearic acid are added in three-dimensional motion mixer, is allowed to and foregoing just mixed powder Continue to mix more than 2h, obtain mixed-powder；Wherein, to account for whole lutetium oxide powder total with magnesium oxide powder for stearic addition The 0.2-0.8% of quality；
(4) cold moudling, dwell time 30-120s, system are carried out to the mixed-powder using 300~600MPa pressure Into target piece pellet green compact；
(5) under the conditions of protective atmosphere, obtained target piece pellet green compact are sintered using non-pressure sintering technology, are burnt Junction temperature is 1550~1850 DEG C, and lutetium oxide target piece pellet is obtained.
The protective atmosphere can use inert gas shielding or vacuum protection.
The protective atmosphere is preferably Ar-5vol%H2Restitutive protection's atmosphere.
Obtained lutetium oxide target piece pellet of the invention belongs to ceramic pellet, and it contains the magnesia for accounting for gross mass 1-10%. In fact, pure zirconia neptunium ceramics can irradiate generation as target piece in reactor238Pu, but because its chemical stability is too high, Therefore being difficult to after irradiation will by chemical treatment238Pu is extracted.Therefore, the present invention attempt by doping second mutually so that Obtained lutetium oxide target piece pellet is easy to extract generation by appropriate chemical treatment238Pu, while improving other pertinences Energy.
By substantial amounts of experiment, inventor has found that the lutetium oxide ceramics for mixing small amounts magnesium can easily pass through nitric acid Chemolysis is carried out, and with preferable dissolution velocity, is easy to238The extraction of Pu.At the same time, this small amount of doping magnesia Lutetium oxide ceramics also have following excellent characteristic concurrently：First, compared to pure zirconia neptunium ceramics, it has more excellent thermal conductivity. The lutetium oxide ceramics of doping magnesia of the invention a small amount of, its room temperature thermal conductivity up to 10-20W/mK, compared with the room of pure zirconia neptunium ceramics Warm conductance 8-10W/mK have significant increase, be thus advantageous to reduce target piece running temperature in heap, mitigate target piece pellet with Cladding interaction, improves safety in operation in target piece heap.2nd, because the thermal neutron absorption cross section of magnesia is very low, therefore its With pile neutron utilization rate higher.3rd, pellet relative density obtained in small amounts magnesium is mixed up to 89%, with pure oxygen The relative density that change neptunium ceramic pellet is typically only 80% or so is compared, and is not reduced not only, is increased on the contrary, is significantly improved Overall neptunium useful load.
In sum, lutetium oxide target piece pellet preparation technology of the invention has technological process relatively simple, and cost is low Advantage, obtained lutetium oxide target piece pellet totality neptunium useful load is high, and neutron utilization rate is high, and possesses higher heat-conductivity, in heap Internal irradiation performance is more preferable, generation238Pu is easy to chemolysis to extract, and with extraction efficiency higher.Using system of the invention Standby technique prepares lutetium oxide target piece pellet, and then produces238Pu fuel, its overall manufacturing cost is relatively low, it is adaptable to238Pu fuel Large-scale production.
Specific embodiment
Embodiments of the present invention are described further with reference to specific embodiment.
Embodiment 1
(1) lutetium oxide powder is taken as needed with magnesium oxide powder as target piece pellet raw material, wherein, magnesium oxide powder Quality account for the 1% of the two gross mass；
(2) in the lutetium oxide powder, the lutetium oxide powder equal with the magnesium oxide powder quality is taken out, will be taken The lutetium oxide powder for going out mixes 6h with the magnesium oxide powder in three-dimensional motion mixer, obtains just mixed powder；
(3) remaining lutetium oxide powder and stearic acid are added in three-dimensional motion mixer, is allowed to and foregoing just mixed powder Continue to mix 3h, obtain mixed-powder；Wherein, stearic addition accounts for whole lutetium oxide powder and magnesium oxide powder gross mass 0.2；
(4) hydraulic press is used in glove box carries out cold moudling with 350MPa pressure to the mixed-powder, during pressurize Between 40s, be made the target piece pellet green compact that relative density is 55%；
(5) under the conditions of protective atmosphere, using non-pressure sintering technology to obtained target piece pellet green sintering 2h, sintering Temperature is 1650 DEG C, and prepared relative density is 85.2% lutetium oxide target piece pellet.
Embodiment 2
(1) lutetium oxide powder is taken as needed with magnesium oxide powder as target piece pellet raw material, wherein, magnesium oxide powder Quality account for the 5% of the two gross mass；
(2) in the lutetium oxide powder, taking-up accounts for the lutetium oxide powder of 0.5 times of the magnesium oxide powder quality, will take The lutetium oxide powder for going out mixes 4h with the magnesium oxide powder in three-dimensional motion mixer, obtains just mixed powder；
(3) remaining lutetium oxide powder and stearic acid are added in three-dimensional motion mixer, is allowed to and foregoing just mixed powder Continue to mix 2h, obtain mixed-powder；Wherein, stearic addition accounts for whole lutetium oxide powder and magnesium oxide powder gross mass 0.4；
(4) hydraulic press is used in glove box carries out cold moudling with 400MPa pressure to the mixed-powder, during pressurize Between 80s, be made the target piece pellet green compact that relative density is 58%；
(5) under the conditions of protective atmosphere, using non-pressure sintering technology to obtained target piece pellet green sintering 3h, sintering Temperature is 1600 DEG C, and prepared relative density is 89% lutetium oxide target piece pellet.
Embodiment 3
(1) lutetium oxide powder is taken as needed with magnesium oxide powder as target piece pellet raw material, wherein, magnesium oxide powder Quality account for the 10% of the two gross mass；
(2) in the lutetium oxide powder, taking-up accounts for the lutetium oxide powder of 4 times of the magnesium oxide powder quality, will take out Lutetium oxide powder mix 8h in three-dimensional motion mixer with the magnesium oxide powder, obtain just mixed powder；
(3) remaining lutetium oxide powder and stearic acid are added in three-dimensional motion mixer, is allowed to and foregoing just mixed powder Continue to mix 5h, obtain mixed-powder；Wherein, stearic addition accounts for whole lutetium oxide powder and magnesium oxide powder gross mass 0.6；
(4) hydraulic press is used in glove box carries out cold moudling with 600MPa pressure to the mixed-powder, during pressurize Between 120s, be made the target piece pellet green compact that relative density is 52%；
(5) under the conditions of protective atmosphere, using non-pressure sintering technology to obtained target piece pellet green sintering 2.5h, burn Junction temperature is 1700 DEG C, and prepared relative density is 81% lutetium oxide target piece pellet.
Embodiment 4
Nitric acid solubility test is carried out to lutetium oxide target piece pellet obtained in embodiment 3, its experiment flow and result are as follows：Will Lutetium oxide target piece pellet is broken into particle, inserts in the concentrated nitric acid solution of 8mol/L, stands 24 hours after stirring, particles in solution Thing substantially completely dissolves.By the solution suction filtration after dissolving, remaining fine particle gross mass is the 4.6% of pellet quality on filter paper, Can accordingly show that pellet dissolution rate is 95.4%.
Result of the test shows there is good chemical solution using lutetium oxide target piece pellet obtained in preparation technology of the invention Xie Xing.

Claims (3)

1. a kind of lutetium oxide target piece pellet preparation technology, it is characterised in that the technique is comprised the following steps：
(1) lutetium oxide powder is taken as needed with magnesium oxide powder as target piece pellet raw material, wherein, the matter of magnesium oxide powder Amount accounts for the 1-10% of the two gross mass；
(2) in the lutetium oxide powder, taking-up accounts for the lutetium oxide powder of 0.5-4 times of the magnesium oxide powder quality, will take out Lutetium oxide powder mix more than 4h in three-dimensional motion mixer with the magnesium oxide powder, obtain just mixed powder；
(3) remaining lutetium oxide powder and stearic acid are added in three-dimensional motion mixer, is allowed to continue with foregoing just mixed powder Mixing more than 2h, obtains mixed-powder；Wherein, stearic addition accounts for whole lutetium oxide powder and magnesium oxide powder gross mass 0.2-0.8%；
(4) cold moudling is carried out to the mixed-powder using 300~600MPa pressure, dwell time 30-120s is made target Part pellet green compact；
(5) under the conditions of protective atmosphere, obtained target piece pellet green compact are sintered using non-pressure sintering technology, sintering temperature It is 1550~1850 DEG C to spend, and lutetium oxide target piece pellet is obtained.
2. lutetium oxide target piece pellet preparation technology as claimed in claim 1, it is characterised in that：The protective atmosphere uses inertia Gas shield or vacuum protection.
3. lutetium oxide target piece pellet preparation technology as claimed in claim 1, it is characterised in that：The protective atmosphere is Ar- 5vol%H2Restitutive protection's atmosphere.
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CN107398553B (en) * 2017-06-20 2019-08-06 中国原子能科学研究院 A kind of Al-NpO2The preparation method of disperse pellet

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