CN106916959B - The method and apparatus of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field - Google Patents
The method and apparatus of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field Download PDFInfo
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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 present invention provides the methods of purification that Solid State Electrotransport under a kind of magnetostatic field prepares high pure rare earth metals, wherein Solid State Electrotransport carries out in the magnetic line of force magnetostatic field parallel with sense of current is applied.In addition, the present invention also provides the devices for implementing this method.Methods and apparatus of the present invention inhibits the vibration of rare earth nuclear heat and electronics in the scattering in non-parallel magnetic field direction, improves the efficiency of Solid State Electrotransport, shortens the purification period of rare earth metal.
Description
Technical field
The invention belongs to metallurgical technology fields;More particularly to a kind of method and apparatus of Purification of Rare Earth Metals, especially one
The method and apparatus of kind of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field.
Background technique
Rare earth is universally acknowledged developing high-tech and national defence sophisticated technology and rebuilds traditional industry indispensable
Strategic resource.Main Countries are using rare earth new material and its related application industry as giving priority to field;And superelevation
Pure rare-earth metals are then the critical materials of above-mentioned new and high technology material original innovation, are the substance bases for researching and developing rare earth new material
Plinth.
The common method of Purification of Rare Earth Metals includes vacuum melting method, vacuum distillation (distillation) method, zone melting method, solid-state
Electromigration, zone refining and Solid State Electrotransport combination method and electrolytic refining process.Rare earth metal is very active, be easy to aoxidize and
Inhale hydrogen, the interstitial impurities such as O, C, S and N for causing some methods of purification to be difficult to effectively remove in rare earth metal;And Solid State Electrotransport
Rodlike rare earth metal is applied constant-direct current electric current to metal under the conditions of high vacuum (or inert atmosphere) by method, utilizes metal itself
Resistance heating to melting temperature below and continue to keep the temperature, can make the interstitial impurities atom such as O, C, S and N in rare earth metal occur
Directional migration, to obtain the rare earth metal of high-purity.
From the 1960s, Iowa State University, U.S. Ames test room and univ cambridge uk's material science
The experimental study of Solid State Electrotransport method Purification of Rare Earth Metals has been carried out at center in succession, is applied with steady to rare earth metal stick in test
DC current obtains the rare earth metals such as purity higher Gd, Tb, Pr, Nd, Er and Dy, but there is current densities for this method
Greatly, the disadvantage of purification time length.
The research report (RI 7480) and United States Patent (USP) US3650931A of U.S. Bureau in 1971 disclose one kind and adopt
The method for carrying out Solid State Electrotransport Purification of Rare Earth Metals with pulse current, in this method, the duty ratio of monophase current is 1:9, can
Pulse current is improved to 3 times or more of steady current.Gold under conditions of same current application time, in La, Ce and Pr
The removal effect for belonging to impurity and nonmetallic inclusion is better than the experiment for applying steady current.
In order to reduce the current density during Solid State Electrotransport, one is disclosed in Chinese patent CN200710047496.8
The method of kind of Electromagnetic heating area smelting refinement metal off field, the core of this method is to apply direction phase to the liquid metal of fusing
Mutually parallel direct current steady current and magnetostatic field make miscellaneous phase metal or alloy ontology under the synergistic effect of magnetic field and electric field
Lower end is purified.The metal molten that this method is purified needed for being made using induction heating, using magnetic field to convection current in metal bath
Inhibiting effect reduce current induced extruding stress effect and caused by convection current, thus improve foreign atom directional migration speed
Degree.In addition, foreign atom is precipitated in the form of phase in the invention, the curvature effect near particle is flowed through using magnetic field and electric current,
Form asymmetric vortex before and after phase particle, the cyclone swabbing effect formed using vortex, driving particle of impurity quickly to
Cathodic migration.It is not to be caused to move by the momentum mass transfer that electronics divides since impurity is to be solid-solubilized in phase particle to migrate, it is required
Electric current significantly reduces, and can achieve the effect that electromigration purifies using lesser current density, current density can be down to 100A/
cm2Below.And non-patent literature 1 (" basic research of the compound electroluminescent phase transition process of parallel magnetic field in alloy graining ", Shanghai
University's master thesis, 2006: 41) it is further noted that only when in melt be precipitated particle after, the electron wind of electric field generation
Can just there be the point of application, and realize the migration of phase particle, if component is that liquid ionic species exists in alloy, can not move
It moves;But influence of the Solid State Electrotransport to gaseous impurity is not inquired into.
In the above method, United States Patent (USP) US3650931A applies pulse current during Solid State Electrotransport, compared to applying
For adding constant direct current, the current density for flowing through metal bar can be improved, improve Solid State Electrotransport rate.Chinese patent
200710047496.8 in the Electromagnetic heating off field method of area smelting refinement metal, applies constant-direct current to liquid metal
Electricity can improve particle of impurity using magnetic field to the inhibiting effect of convection current in metal bath under lesser current density
Directional migration speed, but not electromigration effect of the report this method to the interstitial impurities atom such as O, C and N in metal, this method
Middle metal bar is placed in alundum tube, and metal melting zone may be in contact with alundum tube, especially for the active metals such as rare earth, corundum
Pipe can pollute the metal of required purification.
Summary of the invention
To solve the above-mentioned problems, it is an object of the invention to: a kind of efficient Solid State Electrotransport purification rare earth gold is provided
The method of category and the device for implementing this method.The rare earth metal charge bar for applying Solid State Electrotransport purification is placed in one by the present invention
In a magnetostatic field, the magnetic line of force with apply sense of current it is parallel, using magnetostatic field to rare earth nuclear heat vibrate and
The inhibiting effect of electron scattering significantly improves the migration velocity of the gaseous impurities such as C, N, O and S, to improve purification rare earth gold
The efficiency of category.
The technical solution adopted in the present invention is as follows: a kind of side of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field
Method, which is characterized in that Solid State Electrotransport carries out in the magnetic line of force magnetostatic field parallel with sense of current is applied.
Specifically, preceding method includes the following steps: to vacuumize furnace body, indifferent gas is optionally filled with after vacuumizing
Body;DC power supply is connected, rare earth metal charge bar is heated, is kept the temperature after rising to predetermined temperature;By rare earth metal charge bar
It is placed in the magnetic line of force magnetostatic field parallel with sense of current is applied;Rare earth metal charge bar continued power is heated, reaches pre-
Stop electrified regulation after fixing time, takes out rare earth metal charge bar, the rare earth metal after being purified after cooling.
More specifically, preceding method includes the following steps:
Step 1 increases magnetostatic field using lifting platform, and magnetic field pedestal is made to be higher than observation window;
Rare earth metal charge bar is connected by tantalum connector with positive and negative electrode by step 2, is vacuumized to stainless steel furnace body, or
Inert gas is poured after vacuumizing;
Step 3, anode connect direct current steady power supply or the single-phase DC pulse power with cathode and carry out to rare earth metal charge bar
Heating, is kept the temperature, the temperature of rare earth metal charge bar is measured by infrared radiation thermometer by observation window after rising to predetermined temperature;
Step 4 declines magnetostatic field using lifting platform, and rare earth metal charge bar is made to be located at the center of magnetostatic field;
Step 5 heats rare earth metal charge bar continued power, stops electrified regulation after reaching the predetermined time, after cooling
Take out rare earth metal charge bar, the rare earth metal after being purified.
In preceding method, the rare earth metal is lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium, lutetium, yttrium and scandium.Research
It was found that still in an inert atmosphere, these rare earth metal charge bars are after preceding method is handled, no matter in vacuum atmosphere
It can obtain the higher rare earth metal of purity.
In preceding method, the magnetic induction intensity of the magnetostatic field is 0.01~1.1T, preferably 0.1~1.1T, further
It is preferred that 0.3~1.1T, most preferably 0.5~1.1T.
In preceding method, the temperature of the rare earth metal charge bar is less than its fusing point, is solid-state, temperature in electrotransport process
Degree is 0.5~0.95 times of fusing point, preferably 0.8~0.9 times of fusing point.Impurity after a period of time, inside rare earth metal charge bar
Element redistributes, and can obtain the higher rare earth metal of purity.
In preceding method, the furnace interior pressure range is 10-9~105Pa。
In preceding method, the heating time of the rare earth metal charge bar within the scope of 1~1000h, preferably 50~
Within the scope of 800h, most preferably within the scope of 100~500h.
In preceding method, the current density of the direct current steady power supply is 100~600A/cm2, preferably 200~
500A/cm2, most preferably 250~400A/cm2;The current density of the single-phase DC pulse power is 100~2000A/cm2,
Preferably 500~1800A/cm2, most preferably 1000~1500A/cm2;Frequency be 0.5~10000Hz, preferably 10~
8000Hz, most preferably 100~5000Hz;Duty ratio is 0.1~100%, preferably 1~50%, most preferably 5~20%.
On the other hand, the present invention also provides a kind of devices of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field.
As shown in Figure 1, the device by rare earth metal charge bar 1, tantalum connector 2, ceramic insulation ring 3, anode 4, cathode 5, stainless steel furnace body 6,
Observation window 7, discharge/charge port 8, vacuum system 9, magnetostatic field 10, magnetic field pedestal 11 and lifting platform 12 form;In stainless steel furnace body 6
The upper and lower side of rare earth metal charge bar 1 be connected with anode 4 and the tantalum connector 2 of cathode 5 connect, positive 4 and cathode 5 and constant direct current
Source or the connection of monophasic pulses if DC power supply;Stainless steel furnace body 6 installs observation window 7 and discharge/charge stomata 8, lower end and vacuum system 9
Connection;It is characterized in that, being equipped with a magnetostatic field 10 for surrounding it on the outside of stainless steel furnace body 6,10 lower part of magnetostatic field, which is connected with, to rise
The magnetic field pedestal 11 that drop platform 12 moves up and down.
Compared with the prior art, the advantages of the present invention are as follows:
1, it is ultrahigh vacuum or high-purity inert protective atmosphere in stainless steel furnace body of the invention, oxidizable gold can be purified
Belong to, and avoids the secondary pollution of environment and crucible to metal;
2, Solid State Electrotransport purifying plant is mounted in a magnetostatic field by the present invention, passes through the magnetic parallel with current direction
, it is suppressed that the vibration of rare earth nuclear heat and electronics improve Solid State Electrotransport in the scattering in non-parallel magnetic field direction
Efficiency, shorten the purification period of rare earth metal.
Detailed description of the invention
Fig. 1 is dedicated unit structural schematic diagram of the invention.
Specific embodiment
The invention purpose/or scheme will be provided in the form of preferred embodiment.To the explanation of these embodiments
It is used to help the understanding of the present invention, rather than limits other feasible embodiments, these feasible other embodiments can be by
Practice of the invention is learnt.Electromagnetic heating of the invention is illustrated below with reference to specific embodiment, and solid-state electricity moves off field
The method and apparatus for moving Purification of Rare Earth Metals.
Embodiment 1
The charge bar of diameter 6.8mm, long 150mm is made in metal Nd, is 10 in vacuum degree-6Pa, temperature are 850 DEG C, steady is electric
Current density is 260A/cm2, magnetic induction intensity be 0.5T under conditions of keep the temperature 100h.After Solid State Electrotransport processing, C in Nd charge bar,
O, the gaseous impurities such as N and S element to anode migrate, by cathode terminal C, O, N and S impurity content respectively by 300mg/kg,
250mg/kg, 148mg/kg and 85mg/kg are down to 82mg/kg, 31mg/kg, 46mg/kg and 21mg/kg.
Comparative example 1
The charge bar of diameter 6.8mm, long 150mm is made in metal Nd, is 10 in vacuum degree-6Pa, temperature are 850 DEG C, steady is electric
Current density is 260A/cm2Under the conditions of keep the temperature 100h.After Solid State Electrotransport processing, the gaseous impurities such as C, O, N and S member in Nd charge bar
Element is migrated to anode, by cathode terminal C, O, N and S impurity content respectively by 300mg/kg, 250mg/kg, 148mg/kg and
85mg/kg is down to 194mg/kg, 143mg/kg, 96mg/kg and 54mg/kg.
Embodiment 2
The charge bar of diameter 6.8mm, long 150mm is made in metal Tb, is 10 in vacuum degree-6Pa, temperature are 1150 DEG C, pulse is electric
Stream (duty ratio 10%) density is 1400A/cm2, magnetic induction intensity be 0.5T under conditions of keep the temperature 100h.Solid State Electrotransport processing
Afterwards, in Tb charge bar the gaseous impurities element such as C, O, N and S to anode migrate, by cathode terminal C, O, N and S impurity content respectively by
340mg/kg, 740mg/kg, 130mg/kg and 65mg/kg are down to 43mg/kg, 105mg/kg, 41mg/kg and 27mg/kg.
Comparative example 2
The charge bar of diameter 6.8mm, long 150mm is made in metal Tb, is 10 in vacuum degree-6Pa, temperature are 1150 DEG C, pulse is electric
Stream (duty ratio 10%) density is 1400A/cm2Under conditions of keep the temperature 100h.After Solid State Electrotransport processing, C, O, N in Tb charge bar
It is migrated with gaseous impurities elements such as S to anode, the impurity content by cathode terminal C, O, N and S is respectively by 340mg/kg, 740mg/
Kg, 130mg/kg and 65mg/kg are down to 126mg/kg, 289mg/kg, 85mg/kg and 43mg/kg.
Embodiment 3
The charge bar of diameter 8mm, long 150mm is made in metal Tb, is 10 in vacuum degree-6Pa, temperature are 1150 DEG C, steady current
Density is 358A/cm2, magnetic induction intensity be 0.5T under conditions of keep the temperature 100h.After Solid State Electrotransport processing, C, O in Tb charge bar,
The gaseous impurities such as N and S element is migrated to anode, and the impurity content by cathode terminal C, O, N and S is respectively by 468mg/kg, 620mg/
Kg, 260mg/kg and 85mg/kg are down to 67mg/kg, 84mg/kg, 53mg/kg and 38mg/kg.
Comparative example 3
The charge bar of diameter 8mm, long 150mm is made in metal Tb, is 10 in vacuum degree-6Pa, temperature are 1150 DEG C, steady current
Density is 358A/cm2Under conditions of keep the temperature 100h.After Solid State Electrotransport processing, the gaseous impurities such as C, O, N and S member in Tb charge bar
Element is migrated to anode, by cathode terminal C, O, N and S impurity content respectively by 468mg/kg, 620mg/kg, 260mg/kg and
85mg/kg is down to 143mg/kg, 210mg/kg, 132mg/kg and 63mg/kg.
Embodiment 4
The charge bar of diameter 8mm, long 150mm is made in metal Dy, 3 × 104Pa, temperature are 1050 DEG C, steady current density
For 320A/cm2, magnetic induction intensity be 0.8T under conditions of keep the temperature 300h.After Solid State Electrotransport processing, C, O, N and S in Dy charge bar
Equal gaseous impurities element is migrated to anode, by cathode terminal C, O, N and S impurity content respectively by 340mg/kg, 430mg/kg,
210mg/kg and 70mg/kg are down to 94mg/kg, 67mg/kg, 64mg/kg and 32mg/kg.
Comparative example 4
The charge bar of diameter 8mm, long 150mm is made in metal Dy, 3 × 104Pa, temperature are 1050 DEG C, steady current density
For 320A/cm2Under conditions of keep the temperature 100h.Solid State Electrotransport processing after, in Dy charge bar the gaseous impurities such as C, O, N and S element to
Anode migration, the impurity content by cathode terminal C, O, N and S is respectively by 340mg/kg, 430mg/kg, 210mg/kg and 70mg/kg
It is down to 168mg/kg, 185mg/kg, 95mg/kg and 56mg/kg.
Embodiment 5
The charge bar of diameter 8mm, long 150mm is made in metal Lu, is 6 × 10 in vacuum degree-8Pa, temperature are 1250 DEG C, pulse
Electric current (duty ratio 5%) density is 1800A/cm2, magnetic induction intensity be 1.0T under conditions of keep the temperature 460h.At Solid State Electrotransport
After reason, the gaseous impurities such as C, O, N and S element is migrated to anode in Lu charge bar, and the impurity content by cathode terminal C, O, N and S is distinguished
32mg/kg, 43mg/kg, 46mg/kg and 25mg/kg are down to by 240mg/kg, 860mg/kg, 320mg/kg and 94mg/kg.
Comparative example 5
The charge bar of diameter 8mm, long 150mm is made in metal Lu, is 6 × 10 in vacuum degree-8Pa, temperature are 1250 DEG C, pulse
Electric current (duty ratio 5%) density is 1800A/cm2Under conditions of keep the temperature 460h.After Solid State Electrotransport processing, C, O, N in Lu charge bar
It is migrated with gaseous impurities elements such as S to anode, the impurity content by cathode terminal C, O, N and S is respectively by 240mg/kg, 860mg/
Kg, 320mg/kg and 94mg/kg are down to 68mg/kg, 106mg/kg, 84mg/kg and 63mg/kg.
It can be seen that compared with conventional Solid State Electrotransport method from above-mentioned five groups of check experiment results, electricity of the invention
The method of Solid State Electrotransport Purification of Rare Earth Metals purification effect within the identical purification period is more preferable under magnetic Composite Field, C, O, N and S
Impurity content can reduce at least 76% or more, at least improve 10 percentage points or more than the former.As a whole, the present invention will
Solid State Electrotransport purifying plant is mounted in a magnetostatic field, passes through the magnetic field parallel with current direction, it is suppressed that rare earth metal
Atomic nucleus thermal vibration and electronics improve the efficiency of Solid State Electrotransport, shorten rare earth in the scattering in non-parallel magnetic field direction
The purification period of metal.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of method of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field, which is characterized in that Solid State Electrotransport is in magnetic
It carries out, includes the following steps: in the line of force magnetostatic field parallel with sense of current is applied
Step 1) increases magnetostatic field using lifting platform, and magnetostatic field pedestal is made to be higher than observation window;
Rare earth metal charge bar is connected by tantalum connector with positive and negative electrode by step 2), is vacuumized, is vacuumized to stainless steel furnace body
It is optionally filled with inert gas afterwards;
Step 3), anode connects direct current steady power supply with cathode or the single-phase DC pulse power adds rare earth metal charge bar
Heat is kept the temperature after rising to predetermined temperature, and the temperature of rare earth metal charge bar is measured by infrared radiation thermometer by observation window;
Step 4) declines magnetostatic field using lifting platform, so that rare earth metal charge bar is located at the magnetic line of force equal with sense of current is applied
The center of capable magnetostatic field;
Step 5) heats rare earth metal charge bar continued power, stops electrified regulation after reaching the predetermined time, takes out after cooling dilute
Earth metal charge bar, the rare earth metal after being purified.
2. according to the method described in claim 1, wherein, the rare earth metal be lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium,
Lutetium, yttrium and scandium.
3. according to the method described in claim 1, wherein, the magnetic induction intensity of the magnetostatic field is 0.01~1.1T.
4. according to the method described in claim 1, wherein, the rare earth metal charge bar is solid-state, temperature in electrotransport process
For 0.5~0.95 times of fusing point.
5. according to the method described in claim 1, wherein, the furnace interior pressure range is 10-9~105Pa。
6. according to the method described in claim 1, wherein, the heating time of the rare earth metal charge bar is in 1~1000h range
It is interior.
7. according to the method described in claim 1, wherein, the current density of the direct current steady power supply is 100~600A/cm2;
The current density of the single-phase DC pulse power is 100~2000A/cm2, frequency is 0.5~10000Hz, duty ratio 0.1
~100%.
8. a kind of device of Electromagnetic heating Solid State Electrotransport Purification of Rare Earth Metals off field, the device is by rare earth metal charge bar (1), tantalum
Connector (2), ceramic insulation ring (3), positive (4), cathode (5), stainless steel furnace body (6), observation window (7), discharge/charge port (8), true
Empty set is united (9), the pedestal (11) of the component of the component (10) of generation magnetostatic field, generation magnetostatic field and lifting platform (12) form;No
The upper and lower side of rust steel stove body (6) interior rare earth metal charge bar (1) is connect with the tantalum connector (2) for being connected with positive (4) and cathode (5), just
Pole (4) and cathode (5) are connect with permanent D.C source or monophasic pulses if DC power supply;Stainless steel furnace body (6) installs observation window (7)
With discharge/charge port (8), lower end is connect with vacuum system (9);It is surrounded it is characterized in that, being equipped with one on the outside of stainless steel furnace body (6)
The component (10) of its generation magnetostatic field, component (10) lower part for generating magnetostatic field is connected with and can move down on lifting platform (12) carry out
The pedestal (11) of the component of dynamic generation magnetostatic field.
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Address after: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee after: China Youyan Technology Group Co.,Ltd. Address before: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee before: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee before: GENERAL Research Institute FOR NONFERROUS METALS |
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