CN102240812A - Preparation method for uranium molybdenum alloy powder - Google Patents
Preparation method for uranium molybdenum alloy powder Download PDFInfo
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- CN102240812A CN102240812A CN2011101866205A CN201110186620A CN102240812A CN 102240812 A CN102240812 A CN 102240812A CN 2011101866205 A CN2011101866205 A CN 2011101866205A CN 201110186620 A CN201110186620 A CN 201110186620A CN 102240812 A CN102240812 A CN 102240812A
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- molybdenum alloy
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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
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- Y02E30/00—Energy generation of nuclear origin
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Abstract
The invention provides a preparation method for uranium molybdenum alloy powder, and the method is used for preparing the uranium molybdenum alloy powder meeting the demand on a certain particle size and belongs to the field of nuclear technique application. The preparation method provided by the invention mainly comprises the following steps of: cleaning and activating before activating the uranium molybdenum alloy. By cleaning the uranium molybdenum alloy with aqua regia, distilled water, absolute ether, absolute ethyl alcohol, and the like, an oxide layer on the surface of the uranium molybdenum alloy can be efficiently removed, thereby achieving the clean surface of the uranium molybdenum alloy before absorbing hydrogen. Parameters of an activating process are efficiently controlled, thereby accurately controlling the particle size of the uranium molybdenum alloy powder. The preparation method for the uranium molybdenum alloy powder provided by the invention has the characteristics of less working procedures, simple process, small investment, and the like, and is suitable for being applied to the field of nuclear fuel cycle.
Description
Technical field
The invention belongs to the nuclear material preparing technical field, be specifically related to a kind of preparation method of uranium molybdenum alloy powder, the present invention is used to prepare hybrid reactor porous uranium molybdenum alloy fuel element and prepares required and satisfy the uranium molybdenum alloy powder that certain particle diameter requires.
Background technology
In the natural calculus-dissolving energy exhausted day by day today, nuclear energy has occupied more and more important position.The operation technique of fission nuclear fuel is quite ripe at present, and this wherein is most widely used based on the nuclear fuel of uranium element.Yet common metallic uranium is being the α phase below 668 ℃, and corrosion resistance and anti-radiation performance are all very poor.In order to improve the irradiation stability of fuel, adopt usually in metallic uranium, to add a small amount of alloying element, form the uranium alloy material that acts as a fuel.
At the uranium molybdenum is that γ solid solution occupies very wide temperature range and concentration range in the alloy.Add a certain amount of molybdenum and help that the low temperature direction is stable in opposite directions with the γ of cubic structure, obtain each to same lattice structure, thereby strengthen the anti-radiation performance of uranium.In addition, the uranium molybdenum alloy of certain ingredients can form multiple metastable phase under the specific heat treatment process conditions.In changing the uranium molybdenum alloy, when the content of molybdenum and Technology for Heating Processing, might in very wide scope, change composition, the tissue of phase, and then the physical property and the mechanical property of change alloy, this has important and practical meanings.
At RERTR plan (Reduced Enrichment for Research and Test Reactors, the planning of experiments of reduction research and test reactor fuel enrichment) under the support, the U.S. was from the fuel that begins one's study uranium molybdenum alloy in 1996, leading is Argonne National Laboratory, and Idaho National Laboratory, Oak Ridge National Laboratory, Y-12 factory also have some Fuel Tech. Inc. that participation is all arranged.Early stage research starts from the design and the checking of alloying component.Through the analysis of irradiation examination and other means, the goal in research to dispersion fuel was locked as U-7Mo and U-10Mo gradually afterwards.Russia, France, Argentina, Korea S etc. have also all carried out the research of uranium molybdenum alloy as reactor fuel subsequently.
The preparation of dispersion fuel with uranium fuel material powder as the basis.The efflorescence technology of the uranium dioxide of using in the tradition nuclear power industry and the inter-metallic compound material of uranium is comparatively ripe.Their mechanical milling methods that adopt because they are generally more crisp, get up to have no difficulty so grind more.But this technology is difficult to be applied directly in the powder preparation of uranium molybdenum alloy fuel material, and a most important reason is exactly, and the uranium molybdenum alloy shows very strong metalline, and its plasticity is more much better than the inter-metallic compound material of uranium dioxide and uranium.Proposed hydrogenation dehydriding and atomization afterwards again gradually, back two kinds of methods are owing to introducing the less advantage that has more of impurity.
Atomization comprises the jet atomization method, the centrifugal atomizing method, and rotation electrode atomization etc., its principle is by mechanical means molten alloy to be separated cooling to form spherical powder.In the atomization method of having studied, the most successful with the centrifugal atomizing technology of Korea S's exploitation
[1]The concrete grammar of this technology is as follows: the metal uranium button and the molybdenum piece (U-2Mo and U-10Mo have been used in initial research) that will design proportioning place the graphite crucible that has applied refractory ceramics, use induction melting.Melt metal liquid is poured on the argon atmospher protection graphite disk that rotates at full speed down by an aperture.Drop is subjected to centrifugal action to disperse to fly out curing, falls subsequently in the funnel-form collecting tank of container bottom.In the experimentation, the rotary speed of rate of feeding and disk is most important for the control of finished product powder size and dimension, need be adjusted to suitable parameters to optimize powder morphology.The outstanding advantage of this method is that the gained powder is approximately sphere, smooth surface, but this method initial investment is huge.
As far back as the fifties in last century, the hydrogenation method of dehydrogenating just is employed the production with the metallic uranium powder, and this method is considered to the method for a kind of extraordinary preparation ultra-fine (generally below 38 μ m) powder.Its technological process is as follows: uranium molybdenum alloy block is heated (generally be lower than 300 ℃) under suitable temperature uranium meeting and hydrogen reaction, the hydride density (10.9g/cm of uranium under nitrogen atmosphere
3) than metallic uranium density (about 19g/cm
3) much lower, meeting progressively splits away off from block with the form of hydride powder under the stress effect.After hydrogenation is finished, the hydride powder is heated under vacuum, hydrogen can dissociate gradually and emit, and stays the powder of uranium alloy at last.
Under 250 ℃ hydrogenation temperature,
The hydrogen-absorption speed ratio of phase uranium molybdenum alloy
Mutually much lower.By the hydrogenation kinetic curve of different phase structure uranium molybdenum alloys as can be seen, contain
Many more mutually uranium molybdenum alloy hydrogenation is fast more.Therefore, desire obtains by hydrogenization method
Phase uranium molybdenum alloy powder need be taked usually as step: at first alloy is obtained suitable phase structure by heat treatment; Secondly by the efflorescence of hydrogenation dehydrogenation technology; Allow the powder answer be by suitable heat treatment measure at last
Phase.
People such as Argentine Balart described the hydrogenation dehydrogenation technology that they use in detail in one piece of report in 2000.Here they have utilized the uranium molybdenum alloy
The easier characteristic that is hydrogenated mutually, at first with certain heat treatment make the uranium molybdenum alloy (
Phase) separate out at crystal boundary place
Phase is by right
The hydrogenation of phase makes the separately efflorescence between crystal boundary of uranium molybdenum alloy.Behind dehydrogenation, by heat treatment uranium molybdenum alloy powder is replied again
Phase.The uranium molybdenum alloy composition that uses in the experiment is U-7Mo and U-8Mo, and the author thinks that containing the uranium molybdenum alloy of molybdenum between 5 ~ 8% is more suitable in this technology because they with heat treatment take place to
The phase transformation of phase is relatively easy.Can infer a crystal grain of block materials before each particle is equivalent in the powder that obtains by this method.So be easy to expect, can control the size distribution of powder by controlling raw-material grain size.People such as Argentine Balart in 2002 obtain the uranium molybdenum alloy of different grain sizes by heat treatment, and the hydrogenation dehydrogenation obtains powder as stated above then, has realized the rough control that powder size is distributed.
People such as Argentine Pasqualini had also developed another kind of hydrogenation dehydrogenation method in 2002
[7]The places different with top method are that this method does not have before
Heat of transformation processing procedure directly allows metastable state
The alloy hydride of phase.This hydride particle is bigger, thus also need a process of lapping to make it fragmentation, dehydrogenationization then.This technology is become HMD(Hydriding-milling-dehydriding) technology, i.e. hydrogenation-grinding-dehydrogenation technology.HMD technology at first needs one to inhale hydrogen activation process.At first the U-7Mo alloy is heated to 700 ℃ of insulations about 1 hour under 1bar hydrogen pressure.This process has guaranteed that alloy cube matherial can be by uniform hydrogenation, but its mechanism it be unclear that.The residual stress that comes from casting technique is very big to this process influence, is under the situation of compression on the surface especially, and suction hydrogen effect is bad.After this be only formal hydrogenation process, hydrogenation temperature can be between 50 ℃～190 ℃, but the fastest hydrogen-absorption speed occurs in 120 ℃.Hydrogen pressure remains on below the 2atm, and along with the rising of hydrogen pressure, hydrogen-absorption speed also can increase.Under appropriate condition, the fastest hydrogen-absorption speed can reach 1lt/min.kg.The product of this moment is generally the particle about 5mm, and chemical formula can be used MH
3-xExpression, wherein M represents the U-7Mo alloy, x is generally less than 0.5.Because such particle is the hydride phase of fragility, therefore can pass through the further fragmentation of process of lapping.The size distribution of powder can be similar to by the grinding technics parameter and control.For avoiding the spontaneous combustion of hydride, whole technology is carried out (oxygen content is lower than 5%) in the hypoxemia glove box.The dehydrogenation process is carried out under 700 ℃ vacuum atmosphere.It should be noted that before being exposed to powder in the air, carry out a step pre-oxidation passivating process (expose a hour in 25% air, 75% argon gas, 50% air, 50% argon gas exposes a hour again) earlier, in order to avoid unexpected a large amount of oxidations cause spontaneous combustion.
Contemporaneity, Russia is also studied hydrogenation dehydrogenation technology, and what they used is to contain a series of uranium molybdenum alloys of molybdenum amount at 1.9 wt.%～9.5wt.%.Different with Argentine technology, they at first will
The uranium molybdenum alloy of phase is converted into fully by heat treatment
Mutually and
' phase (U
2Mo) duplex structure carries out the hydrogenation dehydrogenationization then, by a quenching process powder is replied at last to be
Phase.Result of study shows that the size distribution of uranium molybdenum alloy powder is relevant with molybdenum content, and along with the rising of molybdenum content, coarse grained share also can increase in the uranium molybdenum alloy powder.If powder particle is too thick, also can do the circulation of hydrogenation dehydrogenationization several times again, particle size can further reduce.Interpolation aluminium and tin will make powder fining more easy in the uranium molybdenum alloy.
By top analysis, we adopt in the powder that the hydrogenation dehydriding prepares metallic uranium powder technical maturity, equipment investment is few and make as can be seen, and to introduce impurity less; Foreign study person's work shows can adopt this method to prepare uranium molybdenum alloy powder, and can obtain the powder body material of varying particle size by the cycle-index of controlling raw-material grain size or hydrogenation dehydrogenation.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of uranium molybdenum alloy powder.
The preparation method of uranium molybdenum alloy powder of the present invention in turn includes the following steps:
1), the cleaning before the activation
Nitric acid and hydrochloric acid are mixed with wang aqueous solution according to the ratio of 1:3, the uranium molybdenum alloy is placed wang aqueous solution, become silvery white by original grey black up to the uranium molybdenum alloy; The taking-up of uranium molybdenum alloy is cleaned with distilled water, absolute ethyl alcohol, absolute ether successively; Under argon shield atmosphere, cleaned uranium molybdenum alloy is transferred in the reactor;
2), the preliminary treatment before the activation of uranium molybdenum alloy
Reactor is evacuated to 50Pa, is heated to 250 ℃ then, is evacuated to 4Pa again and keeps 30min; Uranium molybdenum alloy after the heating is continued to be heated to 650 ℃, continue to be evacuated to 4Pa and keep 1h, be cooled to room temperature;
3), uranium molybdenum alloy powder system is equipped with
The high-purity hydrogen of 0.2MPa～1.0MPa pressure fed step 2 is housed) in the reactor of the uranium molybdenum alloy that preliminary treatment is good; Obtain the hydrogen of uranium molybdenum alloy according to the numerical value change of the pressure sensor of reactor setting,, determine that the uranium molybdenum alloy inhales the cycle-index of putting hydrogen according to required uranium molybdenum alloy granularity requirements.
Cleaning before the activation of uranium molybdenum alloy among the preparation method of the present invention can be removed the impurity on surface effectively, guarantee to have relative clean Surface before the activation of uranium molybdenum alloy, simultaneously, can reduce bibliographical information about carrying out before the activation of uranium molybdenum alloy
In opposite directions
The converting process of phase has reduced the manufacturing cycle of uranium molybdenum alloy powder widely, has simplified activating process, has reduced the cost of preparation uranium molybdenum alloy powder;
Pretreating process before the activation of uranium molybdenum alloy comprises cold degasification, the hot degasification before the activation.By cold/hot degassing processing to laboratory sample, can remove the oxide impurity of uranium molybdenum alloy surface absorption, avoid in heating process, forming oxide, reduce the hydrogen-absorption speed of sample.By hot degassing processing, can remove micro-moisture is inhaled the hydrogen process to the uranium molybdenum alloy influence effectively to laboratory sample.
The uranium molybdenum alloy must keep 30min to hydrogen and the constant temperature that charges into certain pressure in the reactor that fills the uranium molybdenum alloy in advance before inhaling the hydrogen activation and through after the preliminary treatment, can further eliminate the influence that uranium molybdenum alloy surface impurity is equipped with uranium molybdenum alloy powder system.
The invention has the beneficial effects as follows and shortened the production cycle that uranium molybdenum alloy powder system is equipped with, simplified activating process, reduce the preparation cost of uranium molybdenum alloy powder, can control the granularity of uranium molybdenum alloy powder effectively.
The specific embodiment
The preparation method of uranium molybdenum alloy powder of the present invention, its cleaning process is mainly carried out successively by following four steps: 1) uranium molybdenum alloy sample is placed red fuming nitric acid (RFNA) and concentrated hydrochloric acid (volume ratio 1:3) mixed solution, its objective is the oxide layer of removing the surface, this step is relatively more crucial, directly influence the cleaning quality of uranium molybdenum alloy sample, also influence in the subsequent technique uranium molybdenum alloy and whether can inhale the hydrogen activation; 2) the uranium molybdenum alloy sample after the pickling is placed distilled water, its objective is and remove the residual acid solution of uranium molybdenum alloy sample surfaces; 3) the uranium molybdenum alloy sample after the depickling is placed absolute ether, its purpose is removed the moisture on surface; 4) the uranium molybdenum alloy sample with depickling, dehydration places absolute ethyl alcohol, its objective is the greasy dirt of removing the surface; 5) after under the Ar gas shiled uranium molybdenum alloy sample after depickling, dehydration, the de-oiling being placed reactor and carry out sealing, insert on the activation system and carry out subsequent treatment.
Activation system mainly is made of reactor, standard can, gas tank, pressure sensor, valve and data collecting system etc.Whole activating process system before use must be through helium mass spectrum leak detection, leak rate should less than
The main splendid attire of reactor uranium molybdenum alloy to be activated block; Standard can is mainly used in the uranium molybdenum alloy and inhales the quantitatively calibrating put inspiratory capacity and discharge quantity in the hydrogen; Gas tank is mainly used in the collection of gas flow in the deflation course; Pressure sensor is mainly used in the pressure that the uranium molybdenum alloy puts in the hydrogen process in suction and shows and control; Valve is mainly controlled process system; Data collecting system is mainly used in that uranium molybdenum alloy powder system is equipped with the real-time collection of data in the process and the activating process parameter of uranium molybdenum alloy is provided with.
The concrete preparation process of uranium molybdenum alloy powder of the present invention is as follows:
Cleaning before the uranium molybdenum alloy activation provided by the present invention.Its cleaning process is mainly carried out successively by following four steps: 1) uranium molybdenum alloy sample is placed red fuming nitric acid (RFNA) and concentrated hydrochloric acid (volume ratio 1:3) mixed solution, its objective is the oxide layer of removing the surface, this step is relatively more crucial, directly influence the cleaning quality of uranium molybdenum alloy sample, also influence in the subsequent technique uranium molybdenum alloy and whether can inhale the hydrogen activation; 2) the uranium molybdenum alloy sample after the pickling is placed distilled water, its objective is and remove the residual acid solution of uranium molybdenum alloy sample surfaces; 3) the uranium molybdenum alloy sample after the depickling is placed absolute ether, its purpose is removed the moisture on surface; 4) the uranium molybdenum alloy sample with depickling, dehydration places absolute ethyl alcohol, its objective is the greasy dirt of removing the surface; 5) after under the Ar gas shiled uranium molybdenum alloy sample after depickling, dehydration, the de-oiling being placed reactor and carry out sealing, insert on the activation system and carry out subsequent treatment.
Pretreating process before the sample activation directly influences the hydrogen-absorption speed of sample, by experiment, has determined following pretreating process: 1) at room temperature with pump reactor is evacuated to below the 50Pa, its objective is the surperficial adsorbent of removing sample; 2) reactor is heated to 250 ℃ and with pump depletion to the 4Pa and keep 30min, its objective is the removal of carrying out moisture content; 3) sample is continued to be heated to 650 ℃ and be evacuated to below the 4Pa and keep 1h, its purpose mainly is the cubical expansion explosion by sample, removes the oxide of surface trace and exposes unsalted surface, guarantees the quick suction hydrogen of next step sample.
Be provided with four kinds of activating process parameters (seeing Table 1) in the experiment.From hydrogen-absorption speed, under the A condition, uranium molybdenum alloy sample hydrogen-absorption speed is quite slow, and after the activation, the size distribution of sample is with greater than 150
Granule number in the majority, under the condition D, the hydrogen-absorption speed of uranium molybdenum alloy sample is very fast, and the activation after, the size distribution of sample is 100
With 150
Granule number in the majority.
Table 1 cleaning and activation parameter
| Condition | Cleaning | Charge/g | Hydrogen uptake condition | Cycle-index |
| A | Rare nitric acid+water+ether+ethanol | 43 | 0.4MPa; Room temperature | 5 |
| B | Chloroazotic acid+water+ether+ethanol | 100 | 0.5MPa；80℃ | 10 |
| C | Chloroazotic acid+water+ether+ethanol | 120 | 1.0MPa；80℃ | 15 |
| D | Chloroazotic acid+water+ether+ethanol | 150 | 1.0MPa；80℃ | 20 |
Technical process major technique condition
Nitric acid and hydrochloric acid mixed solution: volume ratio: 1:3, temperature: 35 ℃～40 ℃;
Absolute ether: analyze pure, normal temperature;
Absolute ether: analyze pure, normal temperature;
Cold degassing processing: normal temperature, be evacuated to 2～4Pa and keep 30min;
Hot degassing processing: 250 ℃, be evacuated to 2～4Pa and keep 30min;
Pressurize is handled under the hydrogen atmosphere: 650 ℃, be evacuated to 2～4Pa and keep 60min after filling hydrogen 1atm;
The hydrogen circular treatment is put in suction: inhale the hydrogen temperature: normal temperature～80 ℃; Inhale hydrogen pressure: 5atm～10atm; Hydrogen discharging temperature: 500 ℃～600 ℃;
The hydrogen cycle-index is put in suction: can uranium molybdenum alloy powder granularity according to actual needs carry out concrete setting.
Claims (1)
1. the preparation method of a uranium molybdenum alloy powder is characterized in that, described preparation method in turn includes the following steps:
1), the cleaning before the activation
Nitric acid and hydrochloric acid are mixed with wang aqueous solution according to the ratio of 1:3, the uranium molybdenum alloy is placed wang aqueous solution, become silvery white by original grey black up to the uranium molybdenum alloy; The taking-up of uranium molybdenum alloy is cleaned with distilled water, absolute ethyl alcohol, absolute ether successively; Under argon shield atmosphere, cleaned uranium molybdenum alloy is transferred in the reactor;
2), the preliminary treatment before the activation of uranium molybdenum alloy
Reactor is evacuated to 50Pa, is heated to 250 ℃ then, is evacuated to 4Pa again and keeps 30min; Uranium molybdenum alloy after the heating is continued to be heated to 650 ℃, continue to be evacuated to 4Pa and keep 1h, be cooled to room temperature;
3), uranium molybdenum alloy powder system is equipped with
The high-purity hydrogen of 0.2MPa～1.0MPa pressure fed step 2 is housed) in the reactor of the uranium molybdenum alloy that preliminary treatment is good; Obtain the hydrogen of uranium molybdenum alloy according to the numerical value change of the pressure sensor of reactor setting,, determine that the uranium molybdenum alloy inhales the cycle-index of putting hydrogen according to required uranium molybdenum alloy granularity requirements.
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| CN102764894A (en) * | 2012-07-30 | 2012-11-07 | 四川材料与工艺研究所 | Method for preparing high-purity vanadium powder |
| CN103635272A (en) * | 2011-06-23 | 2014-03-12 | 原子能和替代能源委员会 | Powder of an alloy based on uranium and molybdenum in gamma-metastable phase, composition of powders comprising this powder, and uses of said powder and composition |
| CN103706801A (en) * | 2013-12-26 | 2014-04-09 | 四川材料与工艺研究所 | Preparation method of uranium zirconium alloy powder |
| CN105328196A (en) * | 2015-11-02 | 2016-02-17 | 中国核动力研究设计院 | U-Mo alloy powder manufacturing process for controlling nitrogen content |
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| CN103635272A (en) * | 2011-06-23 | 2014-03-12 | 原子能和替代能源委员会 | Powder of an alloy based on uranium and molybdenum in gamma-metastable phase, composition of powders comprising this powder, and uses of said powder and composition |
| CN103635272B (en) * | 2011-06-23 | 2016-06-29 | 原子能和替代能源委员会 | The purposes of the powder based on uranium and the alloy of molybdenum being in γ-metastable phase, the powder composition including this powder and described powder and compositions |
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| CN102764894B (en) * | 2012-07-30 | 2014-10-29 | 四川材料与工艺研究所 | Method for preparing high-purity vanadium powder |
| CN103706801A (en) * | 2013-12-26 | 2014-04-09 | 四川材料与工艺研究所 | Preparation method of uranium zirconium alloy powder |
| CN103706801B (en) * | 2013-12-26 | 2016-05-25 | 四川材料与工艺研究所 | The preparation method of uranium zircaloy powder |
| CN105328196A (en) * | 2015-11-02 | 2016-02-17 | 中国核动力研究设计院 | U-Mo alloy powder manufacturing process for controlling nitrogen content |
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