CN106636703A - Smelting preparation method of high-Mo-content U base alloy - Google Patents
Smelting preparation method of high-Mo-content U base alloy Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
- C22B9/003—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals by induction
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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Abstract
The invention provides a smelting preparation method of high-Mo-content U base alloy. The method firstly uses a non-self-consumption vacuum arc smelting furnace for preparing a U-Mo intermediate alloy, and then, smelts added U blocks in a vacuum induction furnace to dilute the U-Mo intermediate alloy to prepare a U-(16-20)wt% Mo alloy; the U-Mo intermediate alloy comprises the alloy components of: 40-60 wt% of U and 40-60 wt% of Mo; and the U-(16-20)wt% Mo alloy comprises the alloy components of: 80-84 wt% of U, and 16-20 wt% of Mo. The U-Mo intermediate alloy is designed through the components; and high-melting-point Mo is fully fused in depleted uranium base by using non-self-consumption vacuum smelting to obtain an alloy more-sufficient U-Mo intermediate alloy button-shaped sample. The U-Mo intermediate alloy prepared by the method is uniform in chemical components, and is lighter in component segregation phenomenon; and the XRD detects and analyzes the room temperature as stable gamma phase.
Description
Technical field
The invention belongs to nuclear fuel and preparing technical field, and in particular to prepared by a kind of melting of high Mo content U based alloys
Method.
Background technology
In today of fossil energy increasingly depleted, nuclear energy occupies increasingly consequence.The use of fission nuclear fuel
Technology is quite ripe at present, wherein being most widely used based on the nuclear fuel of uranium element.However, common metallic uranium exists
Less than 668 DEG C is α phases, and corrosion resistance and anti-radiation performance are all very poor.As fuel, this is worthless.The metal of γ-phase
Uranium shows isotropic thermal expansion character compared to α-mutually have the ability of more preferably resistance to irradiation effect, is more suitable for
Nuclear fuel.Regrettably, the metallic uranium of γ-phase can not be stable in the presence of relatively low temperature range, and it uses presence as fuel
Significant technology barrier.One method for solving this problem is that γ-mutually stable is made by adding molybdenum and making metallic uranium alloying
To room temperature.U-Mo alloys there is very wide γ alpha regions and the neutron absorption cross-section of Mo is relatively low, do not result in irradiation neutron
The waste in source.Additionally, U-Mo alloys are because simple etc. with high fission atom density, good Flouride-resistani acid phesphatase stability, post processing
It has been considered as current extremely potential new advanced nuclear fuel.Research shows to be produced surely when Mo contents increase to 8%
Determine γ phases, and with the increase of Mo contents, the γ-phase stability of nuclear fuel is stepped up.Due to Mo element fusing points (2610 DEG C)
It is higher, U-Mo alloys homogenization relatively difficult to achieve prepared by current melting, its alloying component major control is in U- (2～12) wt%
Mo.In order to further improve the stability of U-Mo alloys, need to research and develop that a kind of alloying effect is good, the higher U bases of Mo contents are closed
Golden material, the development for new advanced nuclear fuel provides guidance.
The content of the invention
It is an object of the invention to provide a kind of smelting preparation method of high Mo content U based alloys, it realizes high Mo content U
Full and uniformization of based alloy, makes alloy obtain high stability.
To realize goal of the invention, the technical scheme is that：A kind of smelting preparation method of high Mo content U based alloys,
The method prepares U-Mo intermediate alloys first with non-consumable vacuum arc melting furnace, the then melting addition in vaccum sensitive stove
U blocks, are diluted to U-Mo intermediate alloys, prepare U- (16～20) wt%Mo alloys；Described U-Mo intermediate alloys：Alloy into
U contents are divided to be 40～60wt%, Mo contents are 40～60wt%；Described U- (16～20) wt%Mo alloying component U contents are
80～84wt%, Mo content is 16～20wt%.
A kind of smelting preparation method of high Mo content U based alloys as above, the method comprises the steps：
A) non-consumable vacuum arc melting
The U blocks of constant weight are weighed, according still further to U-Mo intermediate alloy proportioning demands Mo grains are weighed；Close in the middle of described U-Mo
Gold：Alloying component U content is 40～60wt%, and Mo contents are 40～60wt%；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Melting output current is 400～500A, 5～8A of stir current, is the uniform of guarantee sample
Property, the abundant melting of high-melting-point Mo is realized, sample needs to stand up repetition melting 3～10 times, and the alloy sample that melting is obtained is knob
Buckle-like；
B) vacuum induction melting
By the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to preparation U- (16～20)
The a certain amount of U blocks that wt%Mo alloys are weighed are put in the lime crucible of vaccum sensitive stove, are incubated at 1350 DEG C～1550 DEG C
0.5h～2h carries out melting, electromagnetic agitation used in fusion process, be then poured in graphite jig at 1300～1500 DEG C into
Ingot；
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, it is 80 that the alloying component for eventually forming is U contents
～84wt%, Mo content is 16～20wt%.
A kind of smelting preparation method of high Mo content U based alloys as above, the graphite jig described in its step b) is applied
There are zirconium oxide and yttria composite coating, i.e., first spray zirconia coating 0.1-0.2mm, then brushed yttria and answer
Close coating 0.1-0.3mm.
A kind of smelting preparation method of high Mo content U based alloys as above, the raw materials used U blocks of the method are low-carbon (LC) U,
C≤100μg/g；Mo grains purity is more than 99.9%.
A kind of smelting preparation method of high Mo content U based alloys as above, the raw materials used U block sizes of the method are
10mm×10mm×10mm。
A kind of smelting preparation method of high Mo content U based alloys as above, the raw materials used Mo particle sizes of the method are
A kind of smelting preparation method of high Mo content U based alloys as above, it will carry out acid before melting to U blocks
Wash, clean 3～8min repeatedly first in nitric acid, 1～5min is then cleaned in ethanol, finally dry up, to remove U blocks surface
Oxide layer.
Effect of the invention is that：The present invention, using non-consumable vacuum melting, is reached by composition design U-Mo intermediate alloy
Abundant meltings of the high-melting-point Mo in depleted uranium base has been arrived, the more sufficient U-Mo intermediate alloys button shape sample of alloy has been obtained.
Add U blocks in vacuum induction melting to be diluted U-Mo intermediate alloy button shape samples, by the application of ceramic crucible, melting
Temperature, temperature retention time, alloy stirring and the alloy smelting process such as pour into a mould and study and define, it is ensured that composition uniform alloy system
It is standby；Obtain a kind of smelting preparation method of high Mo content U based alloys.The U-Mo alloy compositions being prepared by the method for the present invention
Uniformly, component segregation phenomenon is lighter, and it is also stable γ phases that XRD tests and analyzes its room temperature.
Specific embodiment
With reference to specific embodiment a kind of smelting preparation method of high Mo content U based alloys of the present invention is made into
One step is described.
Embodiment 1
A kind of smelting preparation method of high Mo content U based alloys of the present invention, it comprises the steps
Raw material prepares：U blocks are low-carbon (LC) U (C≤100 μ g/g), and size is 10mm × 10mm × 10mm；Mo particle sizes arePurity is 99.95%.
Pickling was carried out to U blocks before melting, clean 5min repeatedly first in nitric acid, then be cleaned in ethanol
3min, finally dries up, to remove the oxide layer on U blocks surface.
A) non-consumable vacuum melting
Prepare U-50wt%Mo intermediate alloys：Weigh the U blocks of 50g, then the Mo grains for weighing 50g；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Vacuum is 1.0 Χ 10-2Pa, melting output current is 500A, stir current 8A, is guarantor
The uniformity of card sample, realizes the abundant melting of high-melting-point Mo, and sample needs to stand up repetition melting 8 times, the alloy that melting is obtained
Sample is button shape；
B) vacuum induction melting
Close by the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to U-20wt%Mo is prepared
The 150g U blocks that gold is weighed are put in the lime crucible of vaccum sensitive stove, and 1.5h is incubated at 1400 DEG C carries out melting, melting
During use electromagnetic agitation, be then poured into ingot in graphite jig at 1350 DEG C；Described graphite jig scribbles zirconium oxide
With yttria composite coating, i.e., zirconia coating 0.1mm is first sprayed, then brushed yttria composite coating 0.2mm.
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, the alloying component for eventually forming is for U contents
80wt%, Mo content is 20wt%.
The U-Mo alloy compositions prepared by the method are uniform, and component segregation phenomenon is lighter, and XRD tests and analyzes its room
Temperature is also stable γ phases.
Embodiment 2
A kind of smelting preparation method of high Mo content U based alloys of the present invention, it comprises the steps
Raw material prepares：U blocks are low-carbon (LC) U (C≤100 μ g/g), and size is 10mm × 10mm × 10mm；Mo particle sizes arePurity is 99.95%.
Pickling was carried out to U blocks before melting, clean 8min repeatedly first in nitric acid, then be cleaned in ethanol
5min, finally dries up, to remove the oxide layer on U blocks surface.
A) non-consumable vacuum melting
Prepare U-60%Mo intermediate alloys：Weigh the U blocks of 40g, then the Mo grains for weighing 60g；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Vacuum is 1.0 Χ 10-2Pa, melting output current is 500A, stir current 5A, is guarantor
The uniformity of card sample, realizes the abundant melting of high-melting-point Mo, and sample needs to stand up repetition melting 10 times, the alloy that melting is obtained
Sample is button shape；
B) vacuum induction melting
Close by the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to U-16wt%Mo is prepared
Gold weighs 275g U blocks and is put in the lime crucible of vaccum sensitive stove, and 0.5h is incubated at 1550 DEG C carries out melting, melting
Electromagnetic agitation used in journey, is then poured into ingot in graphite jig at 1500 DEG C；Described graphite jig scribble zirconium oxide and
Yttria composite coating, i.e., first spray zirconia coating 0.1mm, then has brushed yttria composite coating 0.1mm.
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, the alloying component for eventually forming is for U contents
84wt%, Mo content is 16wt%.
Embodiment 3
A kind of smelting preparation method of high Mo content U based alloys of the present invention, it comprises the steps：
Raw material prepares：U blocks are low-carbon (LC) U (C≤100 μ g/g), and size is 10mm × 10mm × 10mm；Mo particle sizes arePurity is 99.95%.
Pickling was carried out to U blocks before melting, clean 8min repeatedly first in nitric acid, then be cleaned in ethanol
5min, finally dries up, to remove the oxide layer on U blocks surface.
A) non-consumable vacuum melting
Prepare U-60wt%Mo intermediate alloys：Weigh the U blocks of 40g, then the Mo grains for weighing 60g；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Melting output current is 500A, stir current 8A, is the uniformity for ensureing sample, is realized
The abundant melting of high-melting-point Mo, sample needs to stand up repetition melting 9 times, and the alloy sample that melting is obtained is button shape；
B) vacuum induction melting
Close by the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to U-20wt%Mo is prepared
Gold weighs the U blocks of 200g and is put in the lime crucible of vaccum sensitive stove, and 1h is incubated at 1500 DEG C carries out melting, fusion process
Used in electromagnetic agitation, be then poured into ingot in graphite jig at 1450 DEG C；Described graphite jig scribbles zirconium oxide and three
Y 2 O composite coating, i.e., first spray zirconia coating 0.2mm, then has brushed yttria composite coating 0.3mm.
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, the alloying component for eventually forming is for U contents
80wt%, Mo content is 20wt%.
The U-Mo alloy compositions prepared by the method are uniform, and component segregation phenomenon is lighter, and XRD tests and analyzes its room
Temperature is also stable γ phases.
Embodiment 4
A kind of smelting preparation method of high Mo content U based alloys of the present invention, it comprises the steps
Raw material prepares：U blocks are low-carbon (LC) U (C≤100 μ g/g), and size is 10mm × 10mm × 10mm；Mo particle sizes arePurity is 99.95%.
Pickling was carried out to U blocks before melting, clean 3min repeatedly first in nitric acid, then be cleaned in ethanol
1min, finally dries up, to remove the oxide layer on U blocks surface.
A) non-consumable vacuum melting
Prepare U-50wt%Mo intermediate alloys：Weigh the U blocks of 50g, then the Mo grains for weighing 50g；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Vacuum is 1.0 Χ 10-2Pa, melting output current is 450A, stir current 7A, is guarantor
The uniformity of card sample, realizes the abundant melting of high-melting-point Mo, and sample needs to stand up repetition melting 7 times, the alloy that melting is obtained
Sample is button shape；
B) vacuum induction melting
Close by the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to U-18wt%Mo is prepared
Gold weighs certain mass U blocks and is put in the lime crucible of vaccum sensitive stove, and 1h is incubated at 1400 DEG C carries out melting, melting
Electromagnetic agitation used in journey, is then poured into ingot in graphite jig at 1350 DEG C；Described graphite jig scribble zirconium oxide and
Yttria composite coating, i.e., first spray zirconia coating 0.1mm, then has brushed yttria composite coating 0.2mm.
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, the alloying component for eventually forming is for U contents
82wt%, Mo content is 18wt%.
The U-Mo alloy compositions prepared by the method are uniform, and component segregation phenomenon is lighter, and XRD tests and analyzes its room
Temperature is also stable γ phases.
Embodiment 5
A kind of smelting preparation method of high Mo content U based alloys of the present invention, comprises the steps
Raw material prepares：U blocks are low-carbon (LC) U (C≤100 μ g/g), and size is 10mm × 10mm × 10mm；Mo particle sizes arePurity is 99.95%.
Pickling was carried out to U blocks before melting, clean 3min repeatedly first in nitric acid, then be cleaned in ethanol
5min, finally dries up, to remove the oxide layer on U blocks surface.
A) non-consumable vacuum melting
60g U blocks are weighed, according still further to U-Mo intermediate alloy proportioning demands 40g Mo grains are weighed；Close in the middle of described U-Mo
Gold：Alloying component U content is 60wt%, and Mo contents are 40wt%；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Melting output current is 400A, stir current 8A, is the uniformity for ensureing sample, is realized
The abundant melting of high-melting-point Mo, sample needs to stand up repetition melting 5 times, and the alloy sample that melting is obtained is button shape；
B) vacuum induction melting
Close by the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to U-16wt%Mo is prepared
The 150g U blocks that gold is weighed are put in the lime crucible of vaccum sensitive stove, and 2h is incubated at 1350 DEG C carries out melting, melting
Electromagnetic agitation used in journey, is then poured into ingot in graphite jig at 1300 DEG C；
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, the alloying component for eventually forming is for U contents
84wt%, Mo content is 16wt%.
Described graphite jig scribbles zirconium oxide and yttria composite coating, i.e., first spray zirconia coating 0.1mm,
Yttria composite coating 0.1mm has been brushed again.
Embodiment 6
A kind of smelting preparation method of high Mo content U based alloys of the present invention, comprises the steps：
Raw material prepares：U blocks are low-carbon (LC) U (C≤100 μ g/g), and size is 10mm × 10mm × 10mm；Mo particle sizes arePurity is 99.95%.
Pickling was carried out to U blocks before melting, clean 8min repeatedly first in nitric acid, then be cleaned in ethanol
1min, finally dries up, to remove the oxide layer on U blocks surface.
A) non-consumable vacuum melting
The U blocks of 45g are weighed, according still further to U-Mo intermediate alloy proportioning demands the Mo grains of 55g are weighed；Close in the middle of described U-Mo
Gold：Alloying component U content is 45wt%, and Mo contents are 55wt%；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-
Consumable tungsten electrode carries out electric arc melting；Melting output current is 500A, stir current 6A, is the uniformity for ensureing sample, is realized
The abundant melting of high-melting-point Mo, sample needs to stand up repetition melting 6 times, and the alloy sample that melting is obtained is button shape；
B) vacuum induction melting
Close by the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to U-20wt%Mo is prepared
The 175g U blocks that gold is weighed are put in the lime crucible of vaccum sensitive stove, and 1h is incubated at 1550 DEG C carries out melting, melting
Electromagnetic agitation used in journey, is then poured into ingot in graphite jig at 1500 DEG C；
In vacuum induction melting U-Mo intermediate alloys are diluted by U blocks, the alloying component for eventually forming is for U contents
80wt%, Mo content is 20wt%.
Described graphite jig scribbles zirconium oxide and yttria composite coating, i.e., first spray zirconia coating 0.1mm,
Yttria composite coating 0.1mm has been brushed again.
Claims (7)
1. a kind of smelting preparation method of high Mo content U based alloys, it is characterised in that：The method is first with non-consumable vacuum electric
Arc smelting furnace prepares U-Mo intermediate alloys, and then the melting addition U blocks in vaccum sensitive stove, are carried out dilute to U-Mo intermediate alloys
Release, prepare U- (16～20) wt%Mo alloys；
Described U-Mo intermediate alloys：Alloying component U content is 40～60wt%, and Mo contents are 40～60wt%；
Described U- (16～20) wt%Mo alloying components U content is 80～84wt%, and Mo contents are 16～20wt%.
2. a kind of smelting preparation method of high Mo content U based alloys according to claim 1, it is characterised in that the method
Comprise the steps：
A) non-consumable vacuum arc melting
The U blocks of constant weight are weighed, according still further to U-Mo intermediate alloy proportioning demands Mo grains are weighed；Described U-Mo intermediate alloys：
Alloying component U content is 40～60wt%, and Mo contents are 40～60wt%；
The water jacketed copper crucible good U blocks of counterweight and the mixing of Mo grains being fitted in non-consumable vacuum arc melting furnace, using non-consumable
Tungsten electrode carries out electric arc melting；Melting output current is 400～500A, 5～8A of stir current, is the uniformity for ensureing sample,
The abundant melting of high-melting-point Mo is realized, sample needs to stand up repetition melting 5～10 times, and the alloy sample that melting is obtained is button
Shape；
B) vacuum induction melting
By the button shape alloy sample obtained after step a) non-consumable vacuum meltings and according to preparation U- (16～20) wt%Mo
The a certain amount of U blocks that alloy is weighed are put in the lime crucible of vaccum sensitive stove, at 1350 DEG C～1550 DEG C be incubated 0.5h～
2h carries out melting, electromagnetic agitation used in fusion process, is then poured into ingot in graphite jig at 1300～1500 DEG C；
Vacuum induction melting by U blocks by U-Mo intermediate alloys dilute, the alloying component for eventually forming be U contents be 80～
84wt%, Mo content is 16～20wt%.
3. the smelting preparation method of a kind of high Mo content U based alloys according to claim 2, it is characterised in that：Step b)
Described graphite jig scribbles zirconium oxide and yttria composite coating, i.e., first spray 0.1～0.2mm of zirconia coating, then
Brushing has yttria 0.1～0.3mm of composite coating.
4. the smelting preparation method of a kind of high Mo content U based alloys according to claim 2, it is characterised in that：The method
Raw materials used U blocks are low-carbon (LC) U, C≤100 μ g/g；Mo grains purity is more than 99.9%.
5. the smelting preparation method of a kind of high Mo content U based alloys according to claim 4, it is characterised in that：The method
Raw materials used U block sizes are 10mm × 10mm × 10mm.
6. the smelting preparation method of a kind of high Mo content U based alloys according to claim 4, it is characterised in that：The method
Raw materials used Mo particle sizes are
7. the smelting preparation method of a kind of high Mo content U based alloys according to claim 2, it is characterised in that：In melting
Pickling is carried out to U blocks before, clean 3～8min repeatedly first in nitric acid, 1～5min then be cleaned in ethanol, finally
Dry up, to remove the oxide layer on U blocks surface.
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| CN107723554A (en) * | 2017-11-10 | 2018-02-23 | 中国工程物理研究院材料研究所 | A kind of preparation method of uranium niobium molybdenum alloy |
| CN108103327A (en) * | 2017-12-15 | 2018-06-01 | 中国工程物理研究院材料研究所 | A kind of preparation method of homogeneous uranium tungsten alloy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107723625A (en) * | 2017-11-10 | 2018-02-23 | 中国工程物理研究院材料研究所 | A kind of preparation method of U Mo Zr alloys |
| CN107723554A (en) * | 2017-11-10 | 2018-02-23 | 中国工程物理研究院材料研究所 | A kind of preparation method of uranium niobium molybdenum alloy |
| CN107723625B (en) * | 2017-11-10 | 2019-04-16 | 中国工程物理研究院材料研究所 | A kind of preparation method of U-Mo-Zr alloy |
| CN107723554B (en) * | 2017-11-10 | 2019-06-18 | 中国工程物理研究院材料研究所 | A kind of preparation method of uranium niobium molybdenum alloy |
| CN108103327A (en) * | 2017-12-15 | 2018-06-01 | 中国工程物理研究院材料研究所 | A kind of preparation method of homogeneous uranium tungsten alloy |
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