CN105950878B - A kind of effective apparatus and method for removing impurity in uranium metal - Google Patents
A kind of effective apparatus and method for removing impurity in uranium metal Download PDFInfo
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- CN105950878B CN105950878B CN201610261677.XA CN201610261677A CN105950878B CN 105950878 B CN105950878 B CN 105950878B CN 201610261677 A CN201610261677 A CN 201610261677A CN 105950878 B CN105950878 B CN 105950878B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0286—Obtaining thorium, uranium, or other actinides obtaining uranium refining, melting, remelting, working up uranium
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Abstract
The invention discloses a kind of effective apparatus and method for removing impurity in uranium metal, described device includes electron beam furnace and the melting kettle being arranged in the furnace chamber of the electron beam furnace, the melting kettle includes water jacketed copper crucible and is sleeved on the graphite annulus of the water jacketed copper crucible periphery, wherein, the water jacketed copper crucible has melting chamber and the melting chamber is hemispherical.The above method is carried out using above-mentioned effective device for removing impurity in uranium metal, and methods described includes shove charge, preheating, melting, multiple steps such as come out of the stove, and low impurity uranium ingot is finally made.
Description
Technical field
The present invention relates to the technical field of uranium metal purification, more particularly, it is related to miscellaneous in a kind of effectively removal uranium metal
The apparatus and method of matter.
Background technology
Uranium and its alloy make it be sent out in the fields such as Aero-Space, the energy, medical science due to its unique physicochemical properties
Wave more and more important effect.In terms of the energy, nuclear energy turns into China and tackles one of important solutions of energy crisis, passes through
Further investigation to nuclear material turns into the important leverage of support China nuclear power development.But the impurity element meeting in uranium and its alloy
The performance of uranium metal is directly affected, the phenomenons such as stock utilization is low, performance is unstable, corrosion aggravation are caused.What can be consulted is most
The Refining technology of uranium and its alloy is not discussed in detail number document, and the uranium and uranium alloy prepared have impurity concentration
Height, the phenomenon such as performance is unstable.At present, fusion casting is the preferred technique for preparing metal mold nuclear fuel, but general vacuum induction
Or arc melting method is limited by raw material degree of purity, and easily new introducing impurity, the demand of higher purity uranium metal can not be met.
Compared with the methods such as vacuum induction melting, electronic torch melting has the high degree of superheat, vacuum height, smelting time can
The features such as controlling, polluted without crucible.Current electronic torch melting is mainly for metals such as tungsten, molybdenum, tantalum, niobium, zirconium, silicon.High temperature, low-pressure section
Part is the degassing of uranium metal, field trash is decomposed and the physical and chemical process such as floating, element evaporation create good thermodynamics and
Dynamic conditions, so as to obtain high-purity uranium metal.
Although being related to the correlative study of electronic torch melting uranium metal, the not detailed report of refining and purification process
Impurity content is higher in road, metal mold nuclear fuel prepared by vacuum induction melting method, is expected to be greatly reduced using electron beam melting purification
Impurity content, lifts alloy mass, but temporarily do not have correlative study.The electron beam melting purification purification of uranium metal is different from conventional gold
Category, because the particularity of material is needed badly, a kind of process cycle of exploitation is short, the purifying plant that impurity removal is strong, ratio for input and output is high
And method.
The content of the invention
In order to solve problems of the prior art, it is an object of the invention to provide a kind of process cycle is short, impurity is gone
Except the apparatus and method of impurity in effective removal uranium metal that property is strong, ratio for input and output is high.
An aspect of of the present present invention provides a kind of effective device for removing impurity in uranium metal, and described device includes electron beam
Smelting furnace and the melting kettle being arranged in the furnace chamber of the electron beam furnace, the melting kettle include water jacketed copper crucible and
The graphite annulus of the water jacketed copper crucible periphery is sleeved on, wherein, the water jacketed copper crucible has melting chamber and the melting chamber
It is hemispherical.
According to one embodiment of the invention for effectively removing the device of impurity in uranium metal, the depth of the melting chamber is molten
Refine chamber 0.4~0.8 times of radius, the polished processing of inner surface of the melting chamber and surface roughness reaches Ra 0.8, institute
It is 1.5~2.5 times of the depth of melting chamber to state the height of water jacketed copper crucible, and the external diameter of the water jacketed copper crucible is straight with melting chamber
The difference in footpath is 20~50mm.
According to one embodiment of the invention for effectively removing the device of impurity in uranium metal, the water jacketed copper crucible has circle
The profile of cylinder, if the graphite annulus includes the graphite circle that is stacked in the height direction of dried layer and the graphite annulus is higher by water cooling
Along 20~50mm on copper crucible, the graphite circle is spliced by more than two fan-shaped graphite blocks, different layers graphite circle it
Between fan-shaped graphite block dislocation arrangement.
According to one embodiment of the invention for effectively removing the device of impurity in uranium metal, the thickness of the graphite annulus is 20
~50mm, the internal diameter of the graphite annulus is identical with the external diameter of water jacketed copper crucible, and the external diameter of the graphite annulus is the internal diameter of graphite annulus
2~5 times, the content of ashes of the graphite annulus is not more than 0.08% and the porosity is not more than 22%.
Another aspect provides a kind of effective method for removing impurity in uranium metal, using above-mentioned effective removal
The device of impurity is carried out in uranium metal, and the described method comprises the following steps：
A, shove charge：It is fitted into after uranium metal raw material is cleaned in the melting chamber of the water jacketed copper crucible and in water jacketed copper crucible
Periphery is set with graphite annulus；
B, preheating：By electronic torch melting stove evacuation, the high pressure and line of electron gun, regulation electricity are opened under vacuum
The beam spot diameter, of sub- rifle power and electron beam is simultaneously preheated electron beam scanning uranium metal raw material surface, keeps uranium metal raw material
Not by electron-beam melting；
C, melting：Electron gun power is stepped up, stablizes electron gun power after uranium metal raw material is completely melt and is incubated,
Insulation is slow after terminating to be reduced electron gun power and stops beam bombardment；
D, come out of the stove：Dry clean air is passed through into electron beam furnace and furnace atmosphere is replaced, treats that uranium metal raw material is cooled to
Taken out after room temperature and obtain a uranium ingot, the upper surface epidermis for removing a uranium ingot obtains low impurity uranium ingot.
According to one embodiment of the invention for effectively removing the method for impurity in uranium metal, methods described also includes will be described
Low impurity uranium ingot butt end upward again shove charge and repeat step A to D until obtain the purification step of secondary uranium ingot or multiple uranium ingot,
The upper surface epidermis and lower surface epidermis of the secondary uranium ingot or multiple uranium ingot are removed, lower impurity uranium ingot is obtained, wherein, remove
The upper surface epidermis and each 1~5mm of lower surface epidermis of the secondary uranium ingot or multiple uranium ingot.
According to one embodiment of the invention for effectively removing the method for impurity in uranium metal, after vacuumizing, control furnace chamber is true
Reciprocal of duty cycle reaches 5 × 10-2Pa and gun chamber vacuum reaches 2 × 10-3Pa；In fusion process, furnace chamber vacuum is maintained at
10-2~10-3Pa grades and gun chamber vacuum is maintained at 10-3~10-4Pa grades.
According to one embodiment of the invention for effectively removing the method for impurity in uranium metal, in stepb, with 1~5kW/
Min lifting rate adaptation electron gun power adjusts the beam spot diameter, of electron beam and makes itself and uranium metal raw material to 10~30kW
Edge it is tangent, uniform scanning uranium metal raw material surface simultaneously control preheating time be 2~5min.
According to one embodiment of the invention for effectively removing the method for impurity in uranium metal, in step C, electronics is first controlled
The ratio of rifle power (kW) and the radius (mm) of melting chamber is 1:1~2:1, treat that uranium metal raw material is completely melt follow-up high electricity of continuing rising
The sub- rifle power and ratio of radius (mm) for controlling electron gun power (kW) and melting chamber is 3:1~4:1, keep after 2~10min
Reduction electron gun power and adjust electron gun power (kW) and melting chamber radius (mm) ratio to 2:1~3:After 1, insulation 20
With 5~20kW/min rate reduction electron gun power up to stopping beam bombardment after~40min, wherein, control electron beam
Beam spot diameter, be R/4~3R/4, R for water jacketed copper crucible melting chamber radius.
According to one embodiment of the invention for effectively removing the method for impurity in uranium metal, in step D, vent valve is opened
And dry clean air is passed through into furnace chamber, it is 2~8 × 10 to treat furnace chamber vacuum3Vavuum pump is opened after Pa to vacuumize, and treats furnace chamber vacuum
Spend to reopen vent valve after 50~80Pa and continuing to be passed through dry clean air into furnace chamber, blow-on takes out one after 2~4 times repeatedly
Secondary uranium ingot, removes upper surface 1~5mm of epidermis of a uranium ingot.
Compared with prior art, the invention has the advantages that：
(1) dust removal rate is higher：The present invention crosses hot smelting using electron beam and made a return journey except the impurity in uranium metal, twice melting
Impurity content can be significantly decreased, shortens the process time and reduces production cost.It, which compares traditional purifying technique, can reduce work
More than the step of sequence 2, impurity more than 70% in uranium can be reduced by electronic torch melting purification, good process repeatability, technical stability compared with
The utilization rate of high, material is high and each several part composition is more uniform.
(2) application surface is wider：Device in the present invention is made up of water jacketed copper crucible and graphite annulus, can be matched somebody with somebody according to actual conditions
Put the water jacketed copper crucible and graphite annulus of different-diameter plurality of specifications.The mobility of uranium melt is improved using apparatus of the present invention and is changed
Smelting temperature has been apt to it, there is larger gain to purification effect, the different purifications that can not only meet uranium metal is required, are also applied for
The purification of other metals.
Brief description of the drawings
Fig. 1 show it is according to an exemplary embodiment of the present invention it is effective remove uranium metal in impurity device in water-cooled copper earthenware
The structural representation of crucible, the annular cooling water passage not shown in Fig. 1 in water jacketed copper crucible.Wherein, φ 1 is water jacketed copper crucible
Melting chamber diameter, φ 2 is the external diameter of water jacketed copper crucible, and H1 is the melting chamber depth of water jacketed copper crucible, and H2 is water jacketed copper crucible
Highly.
Fig. 2, which is shown, according to an exemplary embodiment of the present invention effective removes in uranium metal graphite annulus in the device of impurity
Structural representation.Wherein, R2 is the inner ring radius of graphite annulus, and R3 is the outer shroud radius of graphite annulus.
Fig. 3 a and Fig. 3 b are respectively illustrated in example 1 to uranium metal raw material using miscellaneous in effective removal uranium metal of the invention
Micro-organization chart before the apparatus and method melting of matter and the micro-organization chart after melting.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification (including any accessory claim, summary and accompanying drawing), except non-specifically is chatted
State, can alternative features equivalent by other or with similar purpose replaced.I.e., unless specifically stated otherwise, each feature
It is an example in a series of equivalent or similar characteristics.
The present invention is actually to carry out melting to uranium metal using the method for electronic torch melting, so as to remove in uranium metal
Impurity.In order that the purpose that the technique of electronic torch melting can be purified with uranium metal matches, one aspect of the present invention is provided
Universality is stronger and is more suitable for the device of uranium metal melting, on the other hand provides specific Refining work for uranium metal
Skill, so as to realize the purification purpose that process cycle is short, impurity removal is strong and ratio for input and output is high.
The structure and principle for removing the device of impurity in uranium metal first effective to the present invention is described in detail below.
Fig. 1 show it is according to an exemplary embodiment of the present invention it is effective remove uranium metal in impurity device in water-cooled copper earthenware
The structural representation of crucible, the annular water-cooling channel not shown in Fig. 1 in water jacketed copper crucible；Fig. 2 is shown according to example of the present invention
In effective removal uranium metal of property embodiment in the device of impurity graphite annulus structural representation.
As depicted in figs. 1 and 2, according to the exemplary embodiment of the present invention, effective dress for removing impurity in uranium metal
Put including electron beam furnace (not shown) and the melting kettle being arranged in the furnace chamber of electron beam furnace, melting kettle includes
Water jacketed copper crucible 1 and the graphite annulus 4 for being sleeved on the periphery of water jacketed copper crucible 1, wherein, water jacketed copper crucible 1 has melting chamber 2 and melted
Refine chamber 2 hemispherical.Preferably, the inner surface of the melting chamber it is polished processing and surface roughness reaches Ra 0.8, i.e., extremely
Ra0.8 is reached less, but the invention is not restricted to this.
Wherein, electron beam furnace of the present invention can use existing typical electrical beamlet smelting furnace, the present invention
Not to this progress concrete restriction.Electron beam furnace be the kinetic energy of high-velocity electrons line is converted under a high vacuum heat energy as
Thermal source is typically made up of the equipment that carries out Metal Melting, typical electron beam furnace 6 parts：1) electron gun：Electron gun is
The heart of electron beam furnace, it includes pipette tips (being typically made up of filament, negative electrode, anode etc.), focus coil and deflection coil
Deng, electron gun by its structure type can be divided into axial rifle (or Pierre's Si rifle), the annular rifle of non-autoacceleration, the annular rifle of autoacceleration and
Horizontal rifle etc., the quantity of electron gun has single rifle, rush-harvesting and rush-planting and multiple gun etc..2) feed system：If raw material is prefabricated from power consumption
During pole, typically using vertical or horizontal power feed mode：If raw material is bits, block or graininess, using feed hopper
Mode.3) ingot casting system：Raised including crystallizer, ingot pulling mechanism and Chu Ding mechanisms.4) vacuum system：Including vacuum pump set, vacuum
Room, vacuum pipe and valve and vacuum measurement system etc..5) power-supply system：Including main power source (electron gun power supply) and control power supply
With operation power etc..6) cooling system：Including whole cooling waters and pipeline valve etc..
Main improvement is to be used as electron beam using the combining structure of water jacketed copper crucible 1 and graphite annulus 4 in the present invention
The melting kettle of smelting furnace.Wherein, water jacketed copper crucible 1 has melting chamber 2 and melting chamber 2 is hemispherical, the earthenware of such a shape
Crucible compensate for the defects such as fluidity of molten in traditional cylindrical crucible is poor, material ingot surface roughness is higher and is easily broken off, can
Uranium metal melting in situ and the more preferable effect of molten bath uniformity are realized, the purification of uranium metal is more suitable for, and can also be according to reality
Border situation configures the water jacketed copper crucible of different-diameter plurality of specifications.Wherein, water jacketed copper crucible 1 has the profile of cylinder.According to
The preferred embodiments of the present invention, the depth H 1 of melting chamber 2 is 0.4~0.8 times of the radius of melting chamber, the height of water jacketed copper crucible 1
Spend the depth H 1 that H2 is melting chamber 2 1.5~2.5 times, the external diameter φ 2 of water jacketed copper crucible 1 and the difference of the diameter phi 1 of melting chamber 2
It is worth for 20~50mm.
The thermo parameters method of electronic torch melting successively decreases from melting chamber center to edge, thus in the present invention melting chamber hemisphere
The temperature homogeneity for being designed to make molten bath of shape is more preferable.The depth H 1 of melting chamber 2 is set to the radius of melting chamber 0.4~
0.8 times, on the one hand in order that the ingot process of coming out of the stove is more prone to, on the other hand because the heat penetration of electron beam is limited, melt
Surface has the temperature field successively decreased to bottom, if the aspect ratio of melting chamber 2 is excessive, (for example melting chamber depth is more than melting chamber radius
0.8 times), then the amount of metal in semi-molten state will increase, in this part metals the volatilization of field trash and floating etc. act on
It will slow down or even disappear.If but too small (such as 0.4 of melting chamber depth less than melting chamber radius of the aspect ratio of melting chamber 2
Times), then molten metal is shallower, and melt has more turbulent flow under electron beam effect, is unfavorable for the less inclusion floating of particle diameter, together
When be also greatly reduced the yield of high-purity uranium metal.In refining, using the density contrast of uranium and non-volatile field trash to realize
Separation in melt, it is often desirable that the field trash that can not be volatilized can segregation be able on melt top layer after coming out of the stove cut off, therefore
There is melting chamber certain depth to be more favorable for floating and the volatilization of field trash, and melting chamber is too shallow or too deep is unfavorable for field trash
Remove.
In addition, the limitation such as height and external diameter of water jacketed copper crucible is primarily due in addition to melting chamber also need to meet annular cold
But the requirement such as the arrangement of water, mechanical property and ease for operation, at the same also need to avoid being punctured by electron beam and excessively it is heavy etc. no
Good technique effect.
In addition, be additionally provided with annular cooling water passage in water jacketed copper crucible 1, with realize in melting chamber molten metal it is cold
But.
According to the present invention, if graphite annulus 4 can include graphite circle and the graphite annulus height that dried layer is stacked in the height direction
Go out water jacketed copper crucible on along 20~50mm, namely graphite annulus 4 can only include one layer of graphite circle, can also include multilayer in height
The graphite circle being stacked on direction is spent, so as to realize required requirement for height.As shown in Fig. 2 each graphite circle in graphite annulus can
To be spliced by more than two fan-shaped graphite blocks 3.Preferably, the dislocation cloth of fan-shaped graphite block 3 between different layers graphite circle
Put.It can effectively alleviate rapid heat cycle around crucible, excessive temperature differentials etc. in the periphery suit laying graphite annulus 4 of water jacketed copper crucible 1
Phenomenon, suitably slows down the loss of beam energy and stable melt temperature field surrounding so that bath surface is heated evenly and carried
The high surface degree of superheat.
According to a preferred embodiment of the invention, the thickness of graphite annulus 4 is 20~50mm, the internal diameter and water-cooled copper of graphite annulus 4
The external diameter φ 2 of crucible 1 is identical, and the external diameter of graphite annulus 4 is 2~5 times of the internal diameter of graphite annulus 4, wherein, the external diameter of graphite annulus 4 is
Twice of the outer shroud radius R3 of the graphite annulus shown in Fig. 2, the internal diameter of graphite annulus 4 is the inner ring half of graphite annulus shown in Fig. 2
Twice of footpath R2.Preferably, the content of ashes of graphite annulus is not more than 0.08% and the porosity is not more than 22%.
Graphite is good fireproof high-temperature resistant material under a high vacuum, easy processing and with low cost, thermal coefficient of expansion it is small and
With good thermal shock resistance, the high-temperature heating of existing electron beam also has water cooling plant around around water jacketed copper crucible, causes it
Temperature field is extremely uneven, and its size is stablized and is difficult to burst apart because of jump in temperature relatively after water jacketed copper crucible suit graphite annulus.
The effect of graphite annulus is mainly：Electronic torch melting purification needs preferable melt superheat degree, but due to the fusing point of uranium
It is relatively low, if beam power add it is excessive, melt splashing situation is serious and power consumption increase, and impurity volatilization is gone under high vacuum high temperature
Except while uranium can also volatilize, beam power is bigger, and temperature is higher, then the loss of uranium also increases.Install additional after graphite annulus and have
There is certain insulation effect, be that can obtain certain bath surface degree of superheat, temperature noted earlier using relatively low beam power
Degree field distribution is successively decreased from the center of melting chamber to edge, if not installing graphite annulus additional, the temperature field at crucible edge is relatively low, heat loss
Increase and the melt temperature difference be bigger, have the bath surface temperature homogeneity of graphite annulus higher under same power situation and the degree of superheat more
Height, considerably increases the capacity usage ratio of electron beam.
The limitation of graphite content (including ash content, porosity) mainly due to when wherein ash content is more under high temperature high vacuum
These ash contents (such as SiO2、Al2O3Deng) a large amount of CO, Si and Al etc. low oxide, many residual air can be released by graphite reduction
The generation of atmosphere is unfavorable for the stabilization of furnace chamber vacuum and the removal of field trash；And its porosity is larger, then graphite surface can be caused to hold
A large amount of foreign gases are easily adsorbed, are equally unfavorable for purification.
The split of graphite annulus is mainly designed in order to be needed to be adjusted and process according to actual process, while convenient peace
Assembly and disassembly.The setting of graphite annulus internal diameter mainly due to：Graphite has certain solubility in liquid uranium, and carbon belongs to miscellaneous
Prime element, if graphite annulus is relatively near apart with melt, may introduce graphite in melt, if graphite annulus is apart from each other with melt,
Then the beneficial effect of graphite annulus will be weakened.The setting of graphite annulus external diameter mainly due to：Graphite annulus with certain width
Better heat preservation, and graphite annulus can limit the splashing scope of melt, it is to avoid on smelt splashes to body of heater.Graphite annulus is high
The setting for going out the height on edge on crucible is that height is too high to be unfavorable for melting in order to obtain the more satisfactory bath surface degree of superheat
To the observation of bath surface situation in journey, and graphite annulus may also produce the escaping gas release increased；Height is too low, melts
Body heat content scatters and disappears too fast, and effect is not notable.
In fact, the device of the present invention can also include being arranged on the graphite annulus heelpiece (not shown) below graphite annulus,
Only need to ensure that the graphite annulus for being sleeved on water jacketed copper crucible periphery can be higher by the upper of water jacketed copper crucible by graphite annulus heelpiece
Along 20~50mm, without require the whole height of graphite annulus higher than on water jacketed copper crucible along 20~50mm.Wherein, adopted
Graphite annulus heelpiece can be with unrestricted choice, and the present invention to this progress concrete restriction, for example, can not used and waved in high vacuum
Relatively low and better heat stability the material of hair property.
Another aspect provides a kind of effective method for removing impurity in uranium metal, it, which is used, above-mentioned effectively goes
Except the device of impurity in uranium metal is carried out, and methods described includes shove charge, preheating, melting, multiple steps such as come out of the stove.
Step A：Shove charge
It is fitted into after uranium metal raw material is cleaned in the melting chamber 2 of water jacketed copper crucible 1 and is set with the periphery of water jacketed copper crucible 1
Graphite annulus 4.
Wherein it is possible to cleaned using alcohol to uranium metal raw material, and uranium metal raw material form can for uranium ingot,
The common material block form such as uranium button.
Step B：Preheating
By electronic torch melting stove evacuation, the high pressure and line of electron gun are opened under vacuum, electron gun work(is adjusted
The beam spot diameter, of rate and electron beam is simultaneously preheated electron beam scanning uranium metal raw material surface, keeps uranium metal raw material not electric
Beamlet melts.
Wherein, after vacuumizing, control furnace chamber vacuum reaches 5 × 10-2Pa and gun chamber vacuum reaches 2 × 10- 3Pa；And in fusion process, furnace chamber vacuum is maintained at 10-2~10-3Pa grades and gun chamber vacuum is maintained at 10-3
~10-4Pa grades.
In this step, with 1~5kW/min lifting rate adaptation electron gun power to 10~30kW, and electronics is adjusted
The beam spot diameter, of beam makes its edge with uranium metal raw material tangent, and uniform scanning uranium metal raw material surface simultaneously controls the preheating time to be
2~5min.
Step C：Melting
Electron gun power is stepped up, stablizes electron gun power after uranium metal raw material is completely melt and is incubated, insulation knot
It is slow after beam to reduce electron gun power and stop beam bombardment.
In this step, the ratio for first controlling electron gun power (kW) and the radius (mm) of melting chamber is 1:1~2:1, treat
Uranium metal raw material is completely melt follow-up high electron gun power of continuing rising and controls the radius (mm) of electron gun power (kW) and melting chamber
Ratio be 3:1~4:1, keep after 2~10min reduction electron gun power and adjust the half of electron gun power (kW) and melting chamber
The ratio in footpath (mm) is to 2:1~3:After 1, after 20~40min of insulation with 5~20kW/min rate reduction electron gun power until
Stop beam bombardment, wherein, the beam spot diameter, for controlling electron beam is R/4~3R/4, and R is the half of the melting chamber of water jacketed copper crucible
Footpath.
Step D：Come out of the stove
Dry clean air is passed through into electron beam furnace and furnace atmosphere is replaced, taken after uranium metal raw material is cooled to room temperature
Go out to obtain a uranium ingot, the upper surface epidermis for removing a uranium ingot obtains low impurity uranium ingot.
In this step, open and furnace chamber vent valve and dry clean air be passed through into furnace chamber, treat furnace chamber vacuum for 2~8 ×
103Vavuum pump is opened after Pa to vacuumize, and is reopened furnace chamber vent valve after furnace chamber vacuum is 50~80Pa and is continued to stove
Interior is passed through dry clean air, and a uranium ingot is taken out in blow-on after 2~4 times repeatedly, removes upper surface 1~5mm of epidermis of a uranium ingot.
Since being opened electron gun heating, be passed through cooling water in water jacketed copper crucible, whole fusion process cooling water not between
Disconnected, melting terminates and stopped after the bombardment of electron beam, and cooling water is also persistently opened, can after bath surface thermometric reaches room temperature
Close cooling water and come out of the stove.
In addition, the method for the present invention also include by low impurity uranium ingot butt end upward again shove charge and repeat step A to D until
The purification step of secondary uranium ingot or multiple uranium ingot is obtained, the upper surface epidermis and lower surface table of secondary uranium ingot or multiple uranium ingot is removed
Skin, obtains lower impurity uranium ingot.Preferably, the upper surface epidermis and lower surface epidermis each 1 of secondary uranium ingot or multiple uranium ingot are removed
~5mm.
Thus, after using the above method and device, melting twice can substantially reduce the impurity content in uranium metal, shorten
Technique simultaneously reduces production cost；It can reduce more than the step of process 2, can be reduced by electronic torch melting purification compared to traditional purifying technique
Impurity more than 70% in uranium, good process repeatability, technical stability are higher, material utilization rate is high and each several part composition is more equal
It is even.
With reference to example, the invention will be further described.
Example 1：
In the device of this example, a diameter of 100mm of melting chamber of the water jacketed copper crucible and external diameter of water jacketed copper crucible is
130mm, the depth of melting chamber is 30mm, and the inside surface roughness of melting chamber is Ra 0.8, and the height of water jacketed copper crucible is 70mm；
The periphery of water jacketed copper crucible is provided with graphite annulus, and it includes two graphite circles and each graphite circle is spliced by two fan-shaped graphite blocks
Form, the thickness of single graphite circle is 20mm, and the internal diameter of graphite annulus is 130mm, and the external diameter of graphite annulus is 390mm, and graphite annulus is high
Go out along 40mm on crucible, the content of ashes of graphite annulus is not more than 0.08% and the porosity is not more than 22%.
Melting purification is carried out according to the following steps：
(1) shove charge：Raw material loads water-cooled copper using the uranium ingot of 1000 μ g/g impurity elements Als of pre- incorporation after alcohol washes
In the melting chamber of crucible；
(2) vacuumize：Vacuumized after charging, control furnace chamber vacuum reaches 5 × 10-2Pa and gun chamber vacuum reaches
2×10-3Pa；Furnace chamber vacuum in control fusion process is maintained at 10-2~10-3Pa grades and gun chamber vacuum are maintained at
10-3~10-4Pa grades；
(3) preheat：The high pressure and line of electron gun are opened, is arrived with 1~5kW/min lifting rate adaptation electron gun power
10~30kW, the beam spot diameter, of adjustment electron beam makes it tangent with uranium ingot edge, and uniform scanning uranium ingot surface is allowed to preheat and protected
Uranium ingot is held not by electron-beam melting, 5min is preheated；
(4) melting：Electron gun power is stepped up to 50~100kW, treats that uranium ingot is completely melt that follow-up high power of continuing rising is arrived
150kW, continuing reduction after 5min, power is to 100kW and is incubated, and the beam spot diameter, of regulation electron beam is 25mm, is incubated after 20min
With 5~20kW/min rate reduction electron gun power until stopping beam bombardment；
(5) come out of the stove：After uranium ingot is cooled to room temperature, furnace chamber vent valve is opened, a certain amount of dry clean air is passed through, treats that furnace chamber is true
Reciprocal of duty cycle is to 8 × 103Open vavuum pump after Pa to vacuumize, after reopening furnace chamber vent valve after vacuum to 50Pa and continue to stove
Interior is passed through dry clean air, and a uranium ingot is taken out in blow-on after so repeatedly 3 times, removes the upper surface epidermis 3mm of a uranium ingot,
Obtain low impurity uranium ingot；
(6) secondary purification：By low impurity uranium ingot butt end shove charge again upward, repeat the above steps (1)~(5), finally goes
Except the secondary each 2mm of uranium ingot upper and lower end face epidermis of gained, lower impurity uranium ingot is obtained.
Example 2：
In the device of this example, a diameter of 100mm of melting chamber of the water jacketed copper crucible and external diameter of water jacketed copper crucible is
130mm, the depth of melting chamber is 30mm, and the inside surface roughness of melting chamber is Ra 0.8, and the height of water jacketed copper crucible is 70mm；
The periphery of water jacketed copper crucible is provided with graphite annulus, and it only includes a graphite circle and is spliced by four fan-shaped graphite blocks, stone
Mo Huan thickness is 30mm, and the internal diameter of graphite annulus is 130mm, and the external diameter of graphite annulus is 650mm, and graphite annulus is higher by edge on crucible
30mm, the content of ashes of graphite annulus is not more than 0.08% and the porosity is not more than 22%.
Carry out according to the following steps：
(1) shove charge：Raw material loads water-cooled copper using the uranium ingot of 1000 μ g/g impurity elements Als of pre- incorporation after alcohol washes
In the melting chamber of crucible；
(2) vacuumize：Vacuumized after charging, control furnace chamber vacuum reaches 5 × 10-2Pa and gun chamber vacuum reaches
2×10-3Pa；Furnace chamber vacuum in control fusion process is maintained at 10-2~10-3Pa grades and gun chamber vacuum are maintained at
10-3~10-4Pa grades；
(3) preheat：The high pressure and line of electron gun are opened, is arrived with 1~5kW/min lifting rate adaptation electron gun power
10~30kW, adjustment lectron beam spot diameter makes it tangent with uranium ingot edge, and uniform scanning uranium ingot surface is allowed to preheat, and keeps
Uranium ingot preheats 3min not by electron-beam melting；
(4) melting：Electron gun power is stepped up to 50~100kW, treats that uranium ingot is completely melt that follow-up high power of continuing rising is arrived
180kW, continues reduction power after 2min and is incubated to 120kW, regulation lectron beam spot diameter is 20mm, be incubated after 30min with 5~
20kW/min rate reduction electron gun power is until stop beam bombardment；
(5) come out of the stove：After uranium ingot is cooled to room temperature, furnace chamber vent valve is opened, a certain amount of dry clean air is passed through, treats that furnace chamber is true
Reciprocal of duty cycle is to 2 × 103Open vavuum pump after Pa to vacuumize, after reopening furnace chamber vent valve after vacuum to 80Pa and continue to stove
Interior is passed through dry clean air, and a uranium ingot is taken out in blow-on after so repeatedly 4 times, removes the upper surface epidermis 2mm of a uranium ingot,
Obtain low impurity uranium ingot；
(6) three purifications：By low impurity uranium ingot shove charge again upward, repeat the above steps (1)~(5) twice, finally go
Except the multiple each 1mm of uranium ingot upper and lower end face epidermis of gained, lower impurity uranium ingot is obtained.
Example 3：
In the device of this example, a diameter of 160mm of melting chamber of the water jacketed copper crucible and external diameter of water jacketed copper crucible is
200mm, the depth of melting chamber is 40mm, and the inside surface roughness of melting chamber is Ra 0.8, and the height of water jacketed copper crucible is 90mm；
The periphery of water jacketed copper crucible is provided with graphite annulus, and it only includes a graphite circle and is spliced by four fan-shaped graphite blocks, stone
Mo Huan thickness is 20mm, and the internal diameter of graphite annulus is 200mm, and the external diameter of graphite annulus is 600mm, and graphite annulus is higher by edge on crucible
20mm, the content of ashes of graphite annulus is not more than 0.08% and the porosity is not more than 22%.
Carry out according to the following steps：
(1) shove charge：Raw material loads water-cooled copper using the uranium ingot of 1000 μ g/g impurity elements Als of pre- incorporation after alcohol washes
In the melting chamber of crucible；
(2) vacuumize：Vacuumized after charging, control furnace chamber vacuum reaches 5 × 10-2Pa and gun chamber vacuum reaches
2×10-3Pa；Furnace chamber vacuum in control fusion process is maintained at 10-2~10-3Pa grades and gun chamber vacuum are maintained at
10-3~10-4Pa grades；
(3) preheat：The high pressure and line of electron gun are opened, is arrived with 1~5kW/min lifting rate adaptation electron gun power
10~30kW, adjustment lectron beam spot diameter makes it tangent with uranium ingot edge, and uniform scanning uranium ingot surface is allowed to preheat, and keeps
Uranium ingot preheats 4min not by electron-beam melting；
(4) melting：Electron gun power is stepped up to 80~160kW, treats that uranium ingot is completely melt that follow-up high power of continuing rising is arrived
260kW, continues reduction power after 2min and is incubated to 180kW, regulation lectron beam spot diameter is 35mm, be incubated after 25min with 5~
20kW/min rate reduction electron gun power is until stop beam bombardment；
(5) come out of the stove：After uranium ingot is cooled to room temperature, furnace chamber vent valve is opened, a certain amount of dry clean air is passed through, treats that furnace chamber is true
Reciprocal of duty cycle is to 8 × 103Open vavuum pump after Pa to vacuumize, after reopening furnace chamber vent valve after vacuum to 50Pa and continue to stove
Interior is passed through dry clean air, and a uranium ingot is taken out in blow-on after so repeatedly 2 times, removes the upper surface epidermis 3mm of a uranium ingot,
Obtain low impurity uranium ingot；
(6) secondary purification：By low impurity uranium ingot butt end shove charge again upward, repeat the above steps (1)~(5), finally goes
Except the secondary each 2mm of uranium ingot upper and lower end face epidermis of gained, lower impurity uranium ingot is obtained.
Fig. 3 a and Fig. 3 b are respectively illustrated in example 1 to uranium metal raw material using miscellaneous in effective removal uranium metal of the invention
Micro-organization chart before the apparatus and method melting of matter and the micro-organization chart after melting.Pass through electronics in comparison diagram 3a, Fig. 3 b
The micro-organization chart of uranium metal understands before and after beam melting, after the method and device using the present invention, the field trash number in uranium metal
Amount and size are obviously reduced, and through electron beam after purification, doped chemical Al content is reduced within 100 μ g/g doping uranium metal, its
Remaining removal of impurity reaches more than 70%.
The invention is not limited in foregoing embodiment.The present invention, which is expanded to, any in this manual to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (9)
1. a kind of effective device for removing impurity in uranium metal, it is characterised in that described device includes electron beam furnace and set
The melting kettle in the furnace chamber of the electron beam furnace is put, the melting kettle includes water jacketed copper crucible and is sleeved on described
The graphite annulus of water jacketed copper crucible periphery, wherein, the water jacketed copper crucible has melting chamber and the melting chamber is hemispherical；Institute
Stating water jacketed copper crucible has the profile of cylinder, if the graphite annulus include the graphite circle that is stacked in the height direction of dried layer and
The graphite annulus be higher by water jacketed copper crucible on along 20~50mm, the graphite circle is by more than two fan-shaped graphite blocks splicings
Into the fan-shaped graphite block dislocation arrangement between different layers graphite circle.
2. effective device for removing impurity in uranium metal according to claim 1, it is characterised in that the depth of the melting chamber
Spend the radius for melting chamber 0.4~0.8 times, the polished processing of the inner surface of the melting chamber and surface roughness reaches Ra
0.8, the height of the water jacketed copper crucible is 1.5~2.5 times of the depth of melting chamber, the external diameter of the water jacketed copper crucible and melting
The difference of the diameter of chamber is 20~50mm.
3. effective device for removing impurity in uranium metal according to claim 1, it is characterised in that the thickness of the graphite annulus
Spend for 20~50mm, the internal diameter of the graphite annulus is identical with the external diameter of water jacketed copper crucible, the external diameter of the graphite annulus is graphite annulus
2~5 times of internal diameter, the content of ashes of the graphite annulus is not more than 0.08% and the porosity is not more than 22%.
4. a kind of effective method for removing impurity in uranium metal, it is characterised in that using any one of claims 1 to 3
Effective removal uranium metal in the device of impurity carry out, and the described method comprises the following steps：
A, shove charge：It is fitted into after uranium metal raw material is cleaned in the melting chamber of the water jacketed copper crucible and in the periphery of water jacketed copper crucible
It is set with graphite annulus；
B, preheating：By electronic torch melting stove evacuation, the high pressure and line of electron gun are opened under vacuum, electron gun is adjusted
The beam spot diameter, of power and electron beam is simultaneously preheated electron beam scanning uranium metal raw material surface, keep uranium metal raw material not by
Electron-beam melting；
C, melting：Electron gun power is stepped up, stablizes electron gun power after uranium metal raw material is completely melt and is incubated, be incubated
It is slow after end to reduce electron gun power and stop beam bombardment；
D, come out of the stove：Dry clean air is passed through into electron beam furnace and furnace atmosphere is replaced, treats that uranium metal raw material is cooled to room temperature
Take out afterwards and obtain a uranium ingot, the upper surface epidermis for removing a uranium ingot obtains low impurity uranium ingot.
5. effective method for removing impurity in uranium metal according to claim 4, it is characterised in that methods described also includes
By the low impurity uranium ingot butt end upward again shove charge and repeat step A to D until obtaining carrying for secondary uranium ingot or multiple uranium ingot
Pure step, removes the upper surface epidermis and lower surface epidermis of the secondary uranium ingot or multiple uranium ingot, obtains lower impurity uranium ingot, its
In, remove the upper surface epidermis and each 1~5mm of lower surface epidermis of the secondary uranium ingot or multiple uranium ingot.
6. effective method for removing impurity in uranium metal according to claim 4, it is characterised in that after vacuumizing, control
Furnace chamber vacuum reaches 5 × 10-2Pa and gun chamber vacuum reaches 2 × 10-3Pa；In fusion process, by furnace chamber vacuum
It is maintained at 10-2~10-3Pa grades and gun chamber vacuum is maintained at 10-3~10-4Pa grades.
7. effective method for removing impurity in uranium metal according to claim 4, it is characterised in that in stepb, with 1
~5kW/min lifting rate adaptation electron gun power is to 10~30kW, and adjusting the beam spot diameter, of electron beam makes itself and uranium golden
The edge for belonging to raw material is tangent, and uniform scanning uranium metal raw material surface simultaneously controls preheating time to be 2~5min.
8. effective method for removing impurity in uranium metal according to claim 4, it is characterised in that in step C, first control
The ratio of electron gun power (kW) processed and the radius (mm) of melting chamber is 1:1~2:1, continue after uranium metal raw material is completely melt
The rise electron gun power and ratio of radius (mm) for controlling electron gun power (kW) and melting chamber is 3:1~4:1, holding 2~
Electron gun power is reduced after 10min and adjusts the ratio of the radius (mm) of electron gun power (kW) and melting chamber to 2:1~3:1
Afterwards, it is incubated after 20~40min with 5~20kW/min rate reduction electron gun power up to stopping beam bombardment, wherein, control
The beam spot diameter, of electron beam processed is R/4~3R/4, and R is the radius of the melting chamber of water jacketed copper crucible.
9. effective method for removing impurity in uranium metal according to claim 4, it is characterised in that in step D, open
Furnace chamber vent valve is simultaneously passed through dry clean air into furnace chamber, and it is 2~8 × 10 to treat furnace chamber vacuum3Vavuum pump is opened after Pa to vacuumize,
Reopen furnace chamber vent valve after furnace chamber vacuum is 50~80Pa and continue to be passed through dry clean air into furnace chamber, repeatedly 2~4
A uranium ingot is taken out in secondary rear blow-on, removes upper surface 1~5mm of epidermis of a uranium ingot.
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| CN106591938A (en) * | 2016-12-29 | 2017-04-26 | 柳州市圣垒贸易有限公司 | Method for refining high-purity metallic uranium |
| CN110699643B (en) * | 2019-11-12 | 2021-11-09 | 中国工程物理研究院材料研究所 | Preparation method of uranium penta-copper monocrystal film and uranium penta-copper monocrystal film |
| CN112095019B (en) * | 2020-08-11 | 2021-07-30 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
| CN112725714B (en) * | 2020-12-04 | 2022-02-18 | 中国工程物理研究院材料研究所 | Method for refining uranium niobium alloy surface inclusions |
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