CN103602836A - Crude rare earth metal purification method in solid phase - Google Patents
Crude rare earth metal purification method in solid phase Download PDFInfo
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- CN103602836A CN103602836A CN201310452144.6A CN201310452144A CN103602836A CN 103602836 A CN103602836 A CN 103602836A CN 201310452144 A CN201310452144 A CN 201310452144A CN 103602836 A CN103602836 A CN 103602836A
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Abstract
The invention discloses a method of removing one or more nonmetal impurity in crude rare earth metal in a solid phase. The method comprises main steps of tightly packaging the crude rare earth metal and a getter directly contacted with the crude rare earth metal by using metal foil, and putting into a heating container; reacting ad a certain temperature after the reaction atmosphere is adjusted with the nonmetal impurity in the crude rare earth metal dispersing into the getter during the heating process so as to achieve an objective of purifying the crude rare earth metal; and separating the getter with the rare earth metal after cooling. The method can effectively remove the nonmetal impurity in the crude rare earth metal in the solid phase, and has low requirements on shapes of and the impurity content of the rare earth metal, and low requirements on system reaction conditions such as the degree of vacuum, temperature, and the like. The method has simple operation and less processes, and has great potential for purifying rare earth metal in a large scale in the industry.
Description
Technical field
The present invention relates to purification of metals field, relate more specifically to a kind of method of removing one or more nonmetallic impuritys under solid phase from thick rare earth metal.
Background technology
In recent years, high pure rare earth metals is widely used in electronic industry, superconductor industry, semi-conductor industry, nuclear industry and other high and advanced industries, and its demand rolls up.But rare earth metal and nonmetallic impurity, as C, H, O, N, F etc., have very strong binding ability, and nonmetallic impurity can have a strong impact on the performances such as the electricity, magnetic of rare earth metal, so rare earth metal purification techniques is the focus that investigators pursue always.
The purification techniques of rare earth metal mainly contains zone melting method, electron-beam process, vacuum distillation method, solid phase electromigration, electrolytic refining process, and the combination of these methods.Wherein under Low Temperature Solid-Phase, the method for Purification of Rare Earth Metals only has solid phase electromigration, and the method is the effective ways of current degree of depth Purification of Rare Earth Metals, and has good effect to removing interstitial impurity and part metals impurity.But not only the production cycle is long for the method, efficiency is extremely low, and too high to the requirement of raw material shape, foreign matter content, operational condition, cannot meet the requirement of batch production, is also only present in laboratory at present.
The method of purifying metals under another conventional solid phase is outer gettering, the method is to utilize the active substance very strong with metallic matrix intermediate gap impurity bonding force that the foreign gas differential pressure drop in system is extremely low, thereby the foreign gas in metallic matrix is separated out, realized the refining effect of metal.The higher VIB, VIIB family element of fusing point but outer gettering is mainly used in purifying, as Nb, V, Ta etc., considerably less to the application of Purification of Rare Earth Metals.
In addition people (the Materials Transactions such as Kamihira, JIM, VOL.34, No.3,1993) attempt using calcium to do reductor Purification of Rare Earth Metals lanthanum, praseodymium, neodymium, gadolinium, terbium and dysprosium, they are placed in rare earth metal in lime crucible together with calcium, are jointly sealed in the iron ware of argon gas atmosphere, heat and keep 850 ℃ of system temperatures and 870 ℃ to surpass 12 hours, whole process middle-weight rare earths is wrapped in the melt and steam of calcium.But experimental result shows, refining effect not obvious at the temperature higher than calcium fusing point, even for rare earth metal Tb and dysprosium, after thermal treatment, in metallic matrix, oxygen level has increase trend.This is probably because the calcium of melting and rare earth form alloy, though like this calcium absorption the impurity oxygen formation calcium oxide in rare earth, impurity oxygen also cannot finally discharge from solid-state rare earth metal.So the outer gettering of liquid phase does not have positive effect to Purification of Rare Earth Metals.
Summary of the invention
The present invention seeks to introduce a kind of method of removing nonmetallic impurity in thick rare earth metal under solid phase.
In order to achieve the above object, technical scheme of the present invention is as follows:
Under solid phase, remove a method for nonmetallic impurity in thick rare earth metal, comprise the following steps:
1) with tinsel, thick rare earth metal is closely wrapped up and being placed in heating container with the getter directly contacting with thick rare earth metal;
2) reaction atmosphere of heating container is adjusted to vacuum or inert atmosphere;
3) at (0.1-1) T
minat temperature, thermal treatment is 1～6000 minute, T
minrefer to the minimum fusing point in thick rare earth metal fusing point and getter fusing point;
4) thick rare earth metal is separated with getter.
Further, described thick rare earth metal comprises one or several in rare earth metal simple substance or alloy.
Rare earth alloy scope is wider, is difficult for listing one by one, conventional rare earth alloy magnetic material samarium iron alloy, and neodymium-iron alloy and Dy-Fe alloy etc., also have hydrogen storage material lanthanum nickel alloy etc.
Further, the nonmetallic impurity in described thick rare earth metal comprises C, H, O, N.
Nonmetallic impurity is mainly present in rare earth metal lattice with the form of interstitial atom, and when thick rare earth metal is solid phase, nonmetallic impurity velocity of diffusion is also obviously greater than the relatively large metallic impurity of atomic radius.
Further, described getter mainly comprises the simple substance of calcium, barium, yttrium, titanium, zirconium or one or several in its alloy.Getter is to the avidity of nonmetallic impurity much larger than to metallic impurity, so getter can be removed the nonmetallic impurity in thick rare earth metal.
Further, step 1) fusing point of described tinsel is higher than step 3) described thermal treatment temp.
Further, step 1) described heating container is tube furnace or vacuum drying oven.
Further, the T step 3)
minrefer to a centigradetemperature (unit be ℃), it refers to the minimum fusing point of thick rare earth metal fusing point and getter fusing point.Thick rare earth metal and getter close contact, in purification process, thick rare earth metal and getter all keep solid-state, and Heating temperature is lower than its fusing point.Because diffusion of contaminants speed under high temperature is very fast, preferentially choose Heating temperature and be not less than 0.5T
min.
Further, step 2), when vacuum atmosphere, vacuum tightness is not higher than 10
3pa, vacuum tightness herein refers to Absolute truth reciprocal of duty cycle.
Further, step 2) under inert atmosphere, preferentially choose rare gas element as protective atmosphere, the pressure range of inert atmosphere is not less than 10
2pa.
Further, heat treatment time needs rate of diffusion at this temperature of size, Heating temperature and impurity per sample and determines, generally at (0.1-1) T
minat temperature, heat treatment time is greater than 1 minute, is less than 6000 minutes.For fully carrying out of purifying, preferentially choose heat treatment time and be greater than 60 minutes, be less than 6000 minutes.
Further, step 4) by thick rare earth metal separated with getter be generally to carry out after it is cooling.
In the present invention, thick rare earth metal can be any shape and size that obtain of processing, as long as it has surface, can contact and purify with getter.
In the present invention, before reaction, the content of nonmetallic impurity should be lower than the content of corresponding impurity during molecular balance under treatment temp in getter, and the amount of getter wants enough greatly, preferentially, and the quality large 10% at least obtaining than Theoretical Calculation.
The present invention can effectively remove the nonmetallic impurity in thick rare earth metal under solid phase, and require very low to the shape of thick rare earth metal, foreign matter content, reaction conditions to system, as also very low in the requirement of vacuum tightness, temperature etc., simple to operate, flow process is few, and the utmost point has the potentiality at industrial a large amount of Purification of Rare Earth Metals.
The mixture that the method also can be used for comprising rare earth metal or the purification of alloy.
The method also can be used for the nonmetallic impurity except C, H, O, N in thick rare earth metal, as F etc.
Embodiment
Below by specific embodiment, further illustrate technical scheme of the present invention, but protection domain is not limited to this.
Embodiment 1
By thick rare earth metal gadolinium to be purified (oxygen level 1600mass ppm, nitrogen content 400mass ppm, hydrogen richness 450mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 8000mass ppm, nitrogen content 1000mass ppm, hydrogen richness 500mass ppm) is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1100 ℃ of Heating temperatures (are equivalent to 0.84T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
1pa, heat-up time 12h.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 30mass ppm, and nitrogen content is down to 40mass ppm, hydrogen richness 10mass ppm.
Embodiment 2
By thick rare earth metal praseodymium (oxygen level 3000mass ppm) to be purified, car becomes the cylinder of diameter 2mm, get length 10mm one.Getting getter calcium (analytical pure) volume is approximately the twice of gadolinium piece, is cut into small pieces some.Gadolinium piece is clipped in the middle of the fritter of calcium, with nickel sheet, closely wraps up, be placed in vacuum drying oven and heat, 700 ℃ of Heating temperatures (are equivalent to 0.83T
min).In in baking oven, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 12h.After reaction, remove the calcium that is wrapped in praseodymium surface, polishing praseodymium piece surface, detects to such an extent that oxygen level is down to about 200mass ppm.
Embodiment 3
By thick rare earth metal gadolinium to be purified (hydrogen richness 450mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter Ti-Zr alloy is sawn into formed objects, gets two.Gadolinium piece is clipped between two blocks of alloys, with nickel sheet, closely wraps up, be placed in vacuum drying oven and heat, 131 ℃ of Heating temperatures (are equivalent to 0.1T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
1pa, heat-up time 24h.After reaction, remove alloy block, polishing gadolinium piece surface, detects to such an extent that hydrogen richness is down to about 80mass ppm.
Embodiment 4
By thick rare earth metal to be purified (oxygen, hydrogen richness are respectively 1600mass ppm and 400mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Thick rare earth metal is mainly comprised of samarium iron alloy and samarium.Get getter Ti alloy and be sawn into formed objects, get two; Getting getter calcium (analytical pure) volume is approximately the twice of gadolinium piece, is cut into small pieces some.Gadolinium piece is clipped between two Ti sheets, in addition several all with calcium piece close contact, with tantalum piece, closely wrap up, be placed in tube furnace and heat, 839 ℃ of Heating temperatures (are equivalent to T
min).In tube furnace, be filled with high-purity argon gas, and sealing, pressure is 10
2pa, soaking time 1min.After reaction, remove Ti piece and calcium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 1550mass ppm, and hydrogen richness is down to 300mass ppm.
Embodiment 5
By thick rare earth metal to be purified (oxygen level 1500mass ppm), car becomes the right cylinder of diameter 2mm, get length and be 10mm one.Thick rare earth metal is mainly comprised of neodymium-iron alloy and neodymium.Getter yttrium (oxygen level 16600mass ppm) is pressed into the thin slice of 1*7*10mm.Yttrium pellet is wrapped in behind neodymium post outside, then with tantalum piece by its tight parcel, fixing, be placed in tube furnace and heat, 700 ℃ of Heating temperatures (are equivalent to 0.69T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 8 * 10
2pa, heat-up time 6h.After reaction, remove yttrium piece, polishing neodymium piece surface, detects to such an extent that oxygen level is down to about 500mass ppm.
Embodiment 6
By thick rare earth metal to be purified (oxygen level 1500mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Thick rare earth metal is mainly comprised of neodymium and terbium.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Neodymium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 700 ℃ of Heating temperatures (are equivalent to 0.69T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
2pa, heat-up time 12h.After reaction, remove yttrium piece, polishing neodymium piece surface, detects to such an extent that oxygen level is down to about 100mass ppm.
Embodiment 7
By thick rare earth metal Tb to be purified (oxygen level 1600mass ppm),, car becomes the right cylinder of diameter 2mm, get length and be 10mm one.Getter yttrium (oxygen level 16600mass ppm) is pressed into the thin slice of 1*7*10mm.Yttrium pellet is wrapped in behind terbium post outside, then with tantalum piece by its tight parcel, fixing, be placed in tube furnace and heat, 800 ℃ of Heating temperatures (are equivalent to 0.59T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 12h.After reaction, remove yttrium piece, polishing terbium piece surface, detects to such an extent that oxygen level is down to about 800mass ppm.
Embodiment 8
By thick rare earth metal Tb to be purified (oxygen level 1600mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Terbium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 900 ℃ of Heating temperatures (are equivalent to 0.66T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10-
1pa, heat-up time 12h.After reaction, remove yttrium piece, polishing terbium piece surface, detects to such an extent that oxygen level is down to about 400mass ppm.
Embodiment 9
By thick rare earth metal gadolinium (oxygen level 1600mass ppm) to be purified, be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1000 ℃ of Heating temperatures (are equivalent to 0.76T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
2pa, heat-up time 12h.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 180mass ppm.
Embodiment 10
By thick rare earth metal gadolinium (oxygen level 1600mass ppm) to be purified, be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1100 ℃ of Heating temperatures (are equivalent to 0.84T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 6h.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 500mass ppm.
Embodiment 11
By thick rare earth metal gadolinium (oxygen level 1600mass ppm) to be purified, be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1100 ℃ of Heating temperatures (are equivalent to 0.84T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, is respectively 12h heat-up time.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is all down to about 150mass ppm.
Embodiment 12
By thick rare earth metal dysprosium to be purified (nitrogen content 600mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter zirconium (nitrogen content 10mass ppm) is sawn into formed objects, gets two.Dysprosium piece is clipped between two zirconiums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1100 ℃ of Heating temperatures (are equivalent to 0.78T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, is respectively 24h heat-up time.After reaction, remove zirconium piece, polishing dysprosium piece surface, detects to such an extent that nitrogen content is down to about 50mass ppm.
Embodiment 13
By thick rare earth metal gadolinium to be purified (oxygen level 1600mass ppm, carbon content 300mass ppm, nitrogen content 400mass ppm, hydrogen richness 450mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter barium (nitrogen content 10mass ppm, hydrogen richness 10mass ppm) and titanium-zirconium alloy (oxygen level 10mass ppm, nitrogen content 10mass ppm, hydrogen richness 10mass ppm) are sawn into formed objects, respectively get two.Gadolinium piece is clipped between barium piece and titanium-zirconium alloy piece, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 700 ℃ of Heating temperatures (are equivalent to 0.96T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, is respectively 18h heat-up time.After reaction, remove barium piece and alloy block, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 900mass ppm, carbon content 60mass ppm, nitrogen content 50mass ppm, hydrogen richness 100mass ppm.
Embodiment 14
By thick rare earth metal gadolinium (oxygen level 1600mass ppm) to be purified, be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1200 ℃ of Heating temperatures (are equivalent to 0.91T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 6h.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 200mass ppm.
Embodiment 15
By thick rare earth metal gadolinium (oxygen level 1600mass ppm) to be purified, be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium (oxygen level 16600mass ppm) is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 1250 ℃ of Heating temperatures (are equivalent to 0.95T
min).In tube furnace, pass into argon gas, pressure is 10
4pa, heat-up time 6h.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 150mass ppm.
Embodiment 16
By thick rare earth metal gadolinium (oxygen level 1600mass ppm) to be purified, be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getting getter barium (analytical pure) volume is approximately the twice of gadolinium piece, is cut into small pieces some.Gadolinium piece is clipped in the middle of the fritter of calcium, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 600 ℃ of Heating temperatures (are equivalent to 0.82T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10Pa, heat-up time 12h.After reaction, remove the barium that is wrapped in gadolinium surface, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 400mass ppm.
Embodiment 17
By thick rare earth metal gadolinium to be purified (oxygen level 1600mass ppm, hydrogen richness 400mass ppm, carbon content 400mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter barium (analytical pure) and titanium (the about 20mass ppm of oxygen level, hydrogen richness 30mass ppm) are cut into small pieces some, two times of left and right of getting the about gadolinium volume of cumulative volume after evenly mixing.Gadolinium piece is clipped in the middle of the fritter of calcium, titanium, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 600 ℃ of Heating temperatures (are equivalent to 0.82T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 24h.After reaction, remove the barium that is wrapped in gadolinium surface, polishing gadolinium piece surface, detects to such an extent that oxygen level is down to about 350mass ppm, and hydrogen richness is down to about 50mass ppm, and carbon content is down to 60mass ppm.
Embodiment 18
By thick rare earth metal gadolinium to be purified (hydrogen richness 450mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter yttrium is sawn into formed objects, gets two.Gadolinium piece is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in vacuum drying oven and heat, 131 ℃ of Heating temperatures (are equivalent to 0.1T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 6000min.After reaction, remove yttrium piece, polishing gadolinium piece surface, detects to such an extent that hydrogen richness is down to about 10mass ppm.
Embodiment 19
By thick rare earth metal gadolinium to be purified (hydrogen richness 450mass ppm, fluorine content 100mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Getter Ti-Zr alloy is sawn into formed objects, gets two.Gadolinium piece is clipped between two blocks of alloys, with nickel sheet, closely wraps up, be placed in vacuum drying oven and heat, 500 ℃ of Heating temperatures (are equivalent to 0.38T
min).In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 3000min.After reaction, remove alloy block, polishing gadolinium piece surface, detects to such an extent that hydrogen richness is down to about 60massppm, and fluorine content is down to 50mass ppm.
Embodiment 20
By thick rare earth metal to be purified (hydrogen richness 450mass ppm, oxygen level 2100mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Thick rare earth metal is mainly comprised of Dy-Fe alloy.Getter yttrium is sawn into formed objects, gets two.Alloy block is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in tube furnace and heat, 750 ℃ of Heating temperatures.In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 720min.After reaction, remove yttrium piece, polishing alloy block surface, detects to such an extent that hydrogen richness is down to about 60mass ppm, and oxygen level is down to 200mass ppm.
Embodiment 21
By thick rare earth metal to be purified (oxygen level 2000mass ppm), be sawn into the rectangular parallelepiped of 2*2*10mm, get one.Thick rare earth metal is mainly by LaNi
5alloy and dysprosium form.Getter yttrium is sawn into formed objects, gets two.Alloy block is clipped between two yttriums, with tantalum piece, closely wraps up, be placed in vacuum drying oven and heat, 350 ℃ of Heating temperatures.In tube furnace, Absolute truth reciprocal of duty cycle is 10
3pa, heat-up time 3000min.After reaction, remove yttrium piece, polishing alloy block surface, detects to such an extent that oxygen level is down to about 160mass ppm.
Claims (8)
1. under solid phase, remove a method for nonmetallic impurity in thick rare earth metal, comprise the following steps:
1) with tinsel, thick rare earth metal is closely wrapped up and being placed in heating container with the getter directly contacting with thick rare earth metal;
2) reaction atmosphere of heating container is adjusted to vacuum or inert atmosphere;
3) at (0.1-1) T
minat temperature, thermal treatment is 1～6000 minute, T
minrefer to the minimum fusing point in thick rare earth metal fusing point and getter fusing point;
4) thick rare earth metal is separated with getter.
2. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that, described thick rare earth metal comprises one or several in rare earth metal simple substance or alloy.
3. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that, described nonmetallic impurity refers to C, H, O, N.
4. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that, step 1) described in, getter contains nonmetallic impurity, and before reaction, nonmetallic impurity content should be lower than the content of its corresponding nonmetallic impurity during molecular balance under treatment temp in getter.
5. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that step 1) described getter is the simple substance of calcium, yttrium, barium, titanium, zirconium or one or several in its alloy.
6. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that step 1) described heating container is tube furnace or vacuum drying oven.
7. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that step 2) described in reaction atmosphere while being vacuum atmosphere, vacuum tightness is not higher than 10
3pa.
8. under solid phase, remove as claimed in claim 1 the method for nonmetallic impurity in thick rare earth metal, it is characterized in that step 2) described in reaction atmosphere while being inert atmosphere, the pressure of inert atmosphere is not less than 10
2pa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082542A (en) * | 2018-02-24 | 2018-12-25 | 虔东稀土集团股份有限公司 | A method of it preparing the vacuum drying oven of high pure metal ytterbium and its prepares high pure metal ytterbium |
| CN113774241A (en) * | 2021-08-18 | 2021-12-10 | 昆明理工大学 | Purification method of lanthanum-cerium alloy |
| CN116121567A (en) * | 2023-02-16 | 2023-05-16 | 中国科学院金属研究所 | Method for removing impurity elements in metal Mn |
-
2013
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| 侯庆烈: "难熔金属的固态精炼提纯", 《稀有金属》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082542A (en) * | 2018-02-24 | 2018-12-25 | 虔东稀土集团股份有限公司 | A method of it preparing the vacuum drying oven of high pure metal ytterbium and its prepares high pure metal ytterbium |
| CN109082542B (en) * | 2018-02-24 | 2019-05-07 | 虔东稀土集团股份有限公司 | A method of it preparing the vacuum drying oven of high pure metal ytterbium and its prepares high pure metal ytterbium |
| CN113774241A (en) * | 2021-08-18 | 2021-12-10 | 昆明理工大学 | Purification method of lanthanum-cerium alloy |
| CN116121567A (en) * | 2023-02-16 | 2023-05-16 | 中国科学院金属研究所 | Method for removing impurity elements in metal Mn |
| CN116121567B (en) * | 2023-02-16 | 2023-10-20 | 中国科学院金属研究所 | Method for removing impurity elements in metal Mn |
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