CN106835205A - Praseodymium neodymium-iron alloy and preparation method thereof - Google Patents
Praseodymium neodymium-iron alloy and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
The invention discloses a kind of praseodymium neodymium-iron alloy, the content of praseodymium neodymium is 0~95wt%, and surplus is the inevitable impurity of iron and total amount less than 0.5wt%, wherein oxygen≤0.01wt%, carbon≤0.01wt%, phosphorus≤0.01wt%, sulphur≤0.005wt%.The invention also discloses a kind of preparation method of praseodymium neodymium-iron alloy.Praseodymium neodymium-iron alloy composition prepared by the present invention is uniform, segregation is small, impurity content is low, rare-earth yield is high, low cost, pollution-free, is applied to rare earth steel middle rare earth high income, effect is significant, is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of rare-earth metal material, specifically, it is related to a kind of praseodymium neodymium-iron alloy and preparation method thereof.
Background technology
At present, steel is the first big structural metallic materials, is widely used in the neck such as building, the energy, transport, Aero-Space
Domain.The application and its research of rare earth in steel have also obtained fast development, and rare earth can play desulfurization, deoxidation, change in adding molten steel
Inclusion morphology etc. is acted on, and can improve plasticity, punching performance, anti-wear performance and the welding performance of steel.Various rare earth steels are such as
Automobile rear-earth steel plate, mould steel, rail etc. have obtained quite varied application.
It is always the emphasis of this research of research work, existing addition side in the Adding Way of rare earth steel production process middle rare earth
The method diversified forms such as including Feed aluminum wire, core-spun yarn, Rare-earth Iron intermediate alloy, current effect it is obvious be to close in the middle of Rare-earth Iron
Golden addition method.Preparing Rare-earth Iron intermediate alloy technology mainly has following a few classes：
(1) miscible method.
Miscible method is also referred to as to the method for mixing, main to utilize electric arc furnaces or intermediate frequency furnace, and rare earth metal and iron is miscible prepared
Alloy.The method is the method for generally using at present, and its technology is simple, polynary intermediate alloy can be obtained or application is closed
Gold, but there is also deficiency：1) rare earth metal easy local concentration in iron liquid is too high, produces segregation；2) the method is used
Raw material is rare earth metal, and especially for centering heavy rare earth metal, preparation technology is complicated, relatively costly；3) smelting temperature is higher, by
In with rare earth metal and pure iron as raw material, smelting temperature requirement is high.
(2) fused salt electrolysis process.
Fused salt electrolysis process prepares Rare-earth Iron intermediate alloy and is mainly using iron consumable cathode method.Such as Chinese patent
CN1827860 discloses a kind of molten-salt electrolysis production Dy-Fe alloy Processes and apparatus, proposes under the high temperature conditions, to be dissolved in fluorination
Dysprosia in thing solution is ionized, and under DC electric field effect, dysprosium ion is separated out on iron cathode surface, is reduced into metal
Dysprosium, dysprosium forms Dy-Fe alloy with ferroalloyization.This method low production cost, process is simple, but there is also following defect：Close
Golden middle rare earth, the fluctuation of iron partition are big, and hardly possible control, distribution error is up to 3%-5%, influences homogeneity of product.
The content of the invention
Technical problem solved by the invention is to provide a kind of praseodymium neodymium-iron alloy and preparation method thereof, and the praseodymium neodymium iron of preparation is closed
Golden composition is uniform, segregation is small, impurity content is low, rare-earth yield is high, low cost, pollution-free, is applied to rare earth steel middle rare earth yield
High, effect is significant, is suitable for large-scale industrial production.
Technical scheme is as follows：
A kind of praseodymium neodymium-iron alloy, it is characterised in that：The content of praseodymium neodymium is 0~95wt%, and surplus is that iron and total amount are less than
The inevitable impurity of 0.5wt%, wherein oxygen≤0.01wt%, carbon≤0.01wt%, phosphorus≤0.01wt%, sulphur≤
0.005wt%.
A kind of preparation method of praseodymium neodymium-iron alloy, including：
In the equipment of electrolysis praseodymium neodium iron intermediate alloy, in praseodymium fluoride neodymium and the fluoride molten salt electrolyte system of lithium fluoride
Under, it is electrolysis raw material with praseodymium neodymium oxide, it is passed through direct current electrolysis and obtains praseodymium neodium iron intermediate alloy；
Using praseodymium neodium iron intermediate alloy and iron as raw material, convert method and prepare praseodymium neodymium-iron alloy using molten；In praseodymium neodymium-iron alloy,
The content of praseodymium neodymium is 0~95wt%, and surplus is the inevitable impurity of iron and total amount less than 0.5wt%, wherein oxygen≤
0.01wt%, carbon≤0.01wt%, phosphorus≤0.01wt%, sulphur≤0.005wt%.
Further：The equipment for being electrolysed praseodymium neodium iron intermediate alloy does electrolytic cell with graphite, and graphite cake is used as anode, iron staff conduct
There is the receiver for containing alloy consumable negative electrode, negative electrode lower section.
Further：Praseodymium neodium iron intermediate alloy melts converts the equipment of praseodymium neodymium-iron alloy for intermediate frequency furnace, molten to convert process in vacuum
Under the conditions of carry out, crucible use rare earth oxide crucible.
Further：Receiver material selection iron, rare earth oxide or boron nitride.
Further：Also include metal praseodymium neodymium or iron during vacuum melts and converts.
Compared with prior art, the technology of the present invention effect includes：The present invention is directed to problems of the prior art, exploitation
Molten-salt electrolysis new technology, the praseodymium neodymium-iron alloy composition of preparation is uniform, segregation is small, impurity content is low, rare-earth yield is high, cost
It is low, pollution-free, rare earth steel middle rare earth high income, effect is significant are applied to, it is suitable for large-scale industrial production.
1st, in the present invention, praseodymium neodymium-iron alloy advantage is：
(1) impurity content is low.
The praseodymium neodymium-iron alloy that the present invention is provided is irony and rare earth due to, as raw material, smelting crucible using pure zirconia praseodymium neodymium
Oxidation material, introduces impurity content few.
(2) composition is uniform, and praseodymium neodymium content is controllable.
Compared with consumable negative electrode, this praseodymium neodymium-iron alloy composition is more uniform, praseodymium for praseodymium neodymium-iron alloy involved in the present invention
Neodymium content is accurately controlled.It was verified that high-performance rare-earth product made from steel can be prepared with alloy of the present invention.
2nd, the preparation method advantage of praseodymium neodymium-iron alloy disclosed by the invention is：
(1) using praseodymium neodymium oxide as electrolysis raw material, so only producing CO, CO in electrolytic process2It is fluorine-containing with minimal amount of
Gas, environmental pollution is small.
(2) using pure iron rod as consumable negative electrode, the praseodymium neodymium-iron alloy that the praseodymium neodymium for separating out forms low melting point with iron is electrolysed, is had
Beneficial to reduction electrolysis temperature.
(3) the praseodymium neodymium-iron alloy that is obtained after vacuum melts and converts of praseodymium neodium iron intermediate alloy that molten-salt electrolysis is obtained is into sub-control
System is accurate, and due to melting under vacuo, rare earth scaling loss is small, and recovery rate is high, product quality is high.
3rd, exploitation and wide market.
With the development of the development of the national economy, in addition to requiring steel and having intensity and toughness high, also require there is good simultaneously
Good decay resistance, this respect rare earth can play a key effect.Rare earth improve the tough of steel, plasticity, heat-resisting oxidation-resistance and
Wearability aspect also plays an important role.China is the big country of output of steel first, in such a field having a large capacity and a wide range, strengthens rare earth
Application be significant.One of limitation rare earth steel industrialization process important factor in order is exactly the addition of rare earth in steel
Mode, the most effective way of research and development is added in the way of Rare-earth Iron intermediate alloy at present.Produced per year with Baogang (group) company
, it is necessary to consume 2.5 ten thousand tons of 10% rare earth ferroalloy, remarkable in economical benefits as a example by 5000000 tons of rare earth steel sheet materials.After the present invention is implemented
On the one hand there is certain facilitation to improving the industrial structure in area, the regional science and technology strength of lifting；On the other hand it is annual to smelt
Rare earth alloy, is all applied in rare earth steel, can not only produce very big economic benefit, can also reverse China's steel situation
Undesirable situation, has a extensive future；An outlet, power-assisted rare-earth trade, steel industry health can be found for Cheap rare-earth
Sustainable development.
Brief description of the drawings
Fig. 1 is the structural representation of electrolysis praseodymium neodium iron intermediate alloy equipment in the present invention；
Fig. 2 is praseodymium neodymium-iron alloy preparation technology flow chart in the present invention.
Specific embodiment
Example embodiment is described more fully with referring now to accompanying drawing.However, example embodiment can be with various shapes
Formula is implemented, and is not understood as limited to implementation method set forth herein；Conversely, thesing embodiments are provided so that the present invention more
Fully and completely, and by the design of example embodiment those skilled in the art is comprehensively conveyed to.
As shown in figure 1, being the structural representation of electrolysis praseodymium neodium iron intermediate alloy equipment in the present invention；As shown in Fig. 2 being this
Praseodymium neodymium-iron alloy preparation technology flow chart in invention.
The equipment of electrolysis praseodymium neodium iron intermediate alloy used in the present invention, its structure includes：Refractory brick 1, iron set 2, rare earth
Oxide crucible 3, praseodymium neodymium-iron alloy 4, positive plate 5, iron cathode 6, electrolyte 7, electrolytic cell 8, heat-insulation layer 9, carbon smash layer 10.
Electrolytic cell 8 is graphite cuvette, is surrounded by carbon successively in the outside of graphite tank and smashes layer 10, heat-insulation layer 9, refractory brick 1, iron set
2；Iron cathode 6 is provided with the middle part of graphite cuvette；In graphite cuvette positive plate 5 is provided with around iron cathode 6；In the bottom of graphite cuvette
The heart is provided with rare earth oxide crucible 3, and rare earth oxide crucible 3 is relative with iron cathode 6.When using, graphite cuvette is built with electrolyte
7, electrolyte 7 is used in praseodymium fluoride neodymium and lithium fluoride molten salt electrolyte, rare earth oxide crucible 3 and fills praseodymium neodymium-iron alloy 4.
Preparation technology for producing the praseodymium neodymium-iron alloy of rare earth steel, comprises the following steps：
Step 1：Electrolytic cell is done with graphite, graphite cake has splendid attire to close as anode, iron staff as consumable negative electrode, negative electrode lower section
The receiver of gold；
Receiver material can be the one kind in iron, rare earth oxide, boron nitride.
Step 2：In the praseodymium fluoride neodymium mixture of neodymium fluoride (praseodymium fluoride) and the fluoride molten salt electrolyte system of lithium fluoride
In, it is electrolysis raw material with the praseodymium neodymium oxide mixture of neodymia (praseodymium oxide), it is passed through direct current electrolysis and obtains being closed in the middle of praseodymium neodymium iron
Gold；
Step 3：Using praseodymium neodium iron intermediate alloy and iron as raw material, satisfactory praseodymium neodymium iron conjunction is prepared using molten method of converting
Gold.
Praseodymium neodium iron intermediate alloy melt convert praseodymium neodymium-iron alloy equipment be intermediate frequency furnace.It is molten to convert process and enter under vacuum
OK, crucible uses rare earth oxide crucible.
In praseodymium neodymium-iron alloy, the content of praseodymium neodymium is 0-95wt%, and surplus is iron and total amount can not keep away less than 0.5wt%
The impurity exempted from, wherein oxygen≤0.01wt%, carbon≤0.01wt%, phosphorus≤0.01wt%, sulphur≤0.005wt%.
Metal detection is tested according to national standards such as GB/T18115.1-2006 using ICP-MS；The detection of C is according to GB/
T12690.13-1990, is tested using High Frequency IR-Absorption Spectrometric method；The test foundation GB/T12690.4-2003 of O, using indifferent gas
Body pulse-infrared method test.The standard deviation S of chemical composition is calculated by below equation：
Wherein XiBe sample chemistry into；X average values are the average of sample n point chemical compositions, n=20 of the present invention.
Embodiment 1
Using the circular graphitic electrolytic cell of Φ 650mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 70mm pure iron rods, average current intensity 4500A, anodic current density 0.8-
1.0A/cm2, cathode-current density 6-9A/cm2, electrolysis temperature maintains 900-1000 DEG C, and continuous electrolysis 360 hours consume oxygen
Change praseodymium neodymium 3046kg, praseodymium neodymium-iron alloy 2710kg is obtained, average praseodymium neodymium content is 90.5%, current efficiency 85%, and rare earth is received
Rate is 94%, and alloying component the results are shown in Table 1.
The praseodymium neodium iron intermediate alloy composition analysis result of table 1/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 90.5 | 9.25 | 0.0085 | 0.0094 | ＜ 0.01 | ＜ 0.005 | 0.011 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 4kg, with addition of iron staff as raw material
14.1kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide crucible, smelting
The praseodymium neodymium ferrous components obtained after refining are shown in Table 2.
The praseodymium neodymium-iron alloy composition analysis result of table 2/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 20.01 | 79.87 | 0.0080 | 0.0095 | ＜ 0.01 | ＜ 0.005 | 0.008 | ＜ 0.005 |
Embodiment 2
Using the circular graphitic electrolytic cell of Φ 650mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 70mm pure iron rods, average current intensity 4000A, anodic current density 0.8-
1.2A/cm2, cathode-current density 5-8A/cm2, electrolysis temperature maintains 950-1050 DEG C, and continuous electrolysis 240 hours consume oxygen
Change praseodymium neodymium 1805kg, praseodymium neodymium-iron alloy 1803kg is obtained, average praseodymium neodymium content is 80.6%, current efficiency 85%, rare-earth yield
It is 94%, alloying component the results are shown in Table 3.
The praseodymium neodium iron intermediate alloy composition analysis result of table 3/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 80.6 | 19.25 | 0.0085 | 0.0094 | ＜ 0.01 | ＜ 0.005 | 0.012 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 6kg, with addition of iron staff as raw material
10.1kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide crucible, smelting
The praseodymium neodymium ferrous components obtained after refining are shown in Table 4.
The praseodymium neodymium-iron alloy composition analysis result of table 4/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 29.98 | 69.74 | 0.0088 | 0.0089 | ＜ 0.01 | ＜ 0.005 | 0.004 | ＜ 0.005 |
Embodiment 3
Using the circular graphitic electrolytic cell of Φ 400mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 50mm pure iron rods, average current intensity 3000A, anodic current density 0.7-
1.1A/cm2, cathode-current density 8-12A/cm2, electrolysis temperature maintains 950-1050 DEG C, and continuous electrolysis 240 hours consume oxygen
Change praseodymium neodymium 1354kg, praseodymium neodymium-iron alloy 1165kg is obtained, average praseodymium neodymium content is 93.6%, current efficiency 85%, and rare earth is received
Rate is 94%, and alloying component the results are shown in Table 5.
The praseodymium neodium iron intermediate alloy composition analysis result of table 5/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 93.6 | 6.15 | 0.0085 | 0.0094 | ＜ 0.01 | ＜ 0.005 | 0.012 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 10kg, with addition of gold as raw material
Category praseodymium neodymium 2.8kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide earthenware
Crucible, the praseodymium neodymium ferrous components obtained after smelting are shown in Table 6.
The praseodymium neodymium-iron alloy composition analysis result of table 6/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 94.97 | 4.91 | 0.0074 | 0.0093 | ＜ 0.01 | ＜ 0.005 | 0.003 | ＜ 0.005 |
Embodiment 4
Using the circular graphitic electrolytic cell of Φ 650mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 80mm pure iron rods, average current intensity 5000A, anodic current density 0.5-
1.0A/cm2, cathode-current density 4-7A/cm2, electrolysis temperature maintains 1000-1070 DEG C, and continuous electrolysis 240 hours consume oxygen
Change praseodymium neodymium 2257kg, praseodymium neodymium-iron alloy 2429kg is obtained, average praseodymium neodymium content is 74.8%, current efficiency 85%, and rare earth is received
Rate is 94%, and alloying component the results are shown in Table 7.
The praseodymium neodium iron intermediate alloy composition analysis result of table 7/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 74.8 | 24.95 | 0.0086 | 0.0093 | ＜ 0.01 | ＜ 0.005 | 0.012 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 15kg, with addition of iron as raw material
Rod 7.4kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide crucible, smelting
The praseodymium neodymium ferrous components obtained after refining are shown in Table 8.
The praseodymium neodymium-iron alloy composition analysis result of table 8/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 49.9 | 49.85 | 0.0077 | 0.0085 | ＜ 0.01 | ＜ 0.005 | 0.0029 | ＜ 0.005 |
Embodiment 5
Using the circular graphitic electrolytic cell of Φ 400mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 45mm pure iron rods, average current intensity 2800A, anodic current density 0.5-
1.0A/cm2, cathode-current density 7-11A/cm2, electrolysis temperature maintains 900-1050 DEG C, and continuous electrolysis 150 hours consume oxygen
Change praseodymium neodymium 790kg, praseodymium neodymium-iron alloy 691kg is obtained, average praseodymium neodymium content is 92%, current efficiency 85%, rare earth recovery rate
94%, alloying component the results are shown in Table 9.
The praseodymium neodium iron intermediate alloy composition analysis result of table 9/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 92.0 | 7.85 | 0.0084 | 0.0095 | ＜ 0.01 | ＜ 0.005 | 0.011 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 1.8kg, with addition of pure as raw material
Iron staff 14.8kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide earthenware
Crucible, the praseodymium neodymium ferrous components obtained after smelting are shown in Table 10.
The praseodymium neodymium-iron alloy composition analysis result of table 10/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 9.93 | 89.76 | 0.0096 | 0.0077 | ＜ 0.01 | ＜ 0.005 | 0.010 | ＜ 0.005 |
Embodiment 6
Using the circular graphitic electrolytic cell of Φ 700mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 60mm pure iron rods, average current intensity 6000A, anodic current density 0.7-
1.1A/cm2, cathode-current density 8-12A/cm2, electrolysis temperature maintains 950-1050 DEG C, and continuous electrolysis 480 hours consume oxygen
Change praseodymium neodymium 5416kg, praseodymium neodymium-iron alloy 4837kg is obtained, average praseodymium neodymium content is 90.2%, current efficiency 85%, and rare earth is received
Rate is 94%, and alloying component the results are shown in Table 11.
The praseodymium neodium iron intermediate alloy composition analysis result of table 11/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 90.2 | 9.54 | 0.0094 | 0.0085 | ＜ 0.01 | ＜ 0.005 | 0.014 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 10kg, with addition of iron as raw material
Rod 5kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide crucible, smelts
The praseodymium neodymium ferrous components for obtaining afterwards are shown in Table 12.
The praseodymium neodymium-iron alloy composition analysis result of table 12/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 60.11 | 39.71 | 0.0071 | 0.0081 | ＜ 0.01 | ＜ 0.005 | 0.003 | ＜ 0.005 |
Embodiment 7
Using the circular graphitic electrolytic cell of Φ 700mm, anode is made up of four pieces of graphite cakes, and praseodymium fluoride neodymium is in electrolyte
85wt%, lithium fluoride are 15wt%, and negative electrode is 75mm pure iron rods, average current intensity 5000A, anodic current density 0.6-
1.0A/cm2, cathode-current density 5-8A/cm2, electrolysis temperature maintains 900-1050 DEG C, and continuous electrolysis 150 hours consume oxygen
Change praseodymium neodymium 1410kg, praseodymium neodymium-iron alloy 1333kg is obtained, average praseodymium neodymium content is 85.2%, current efficiency 85%, and rare earth is received
Rate is 95%, and alloying component the results are shown in Table 13.
The praseodymium neodium iron intermediate alloy composition analysis result of table 13/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 85.2 | 14.54 | 0.0075 | 0.0084 | ＜ 0.01 | ＜ 0.005 | 0.013 | ＜ 0.005 |
The praseodymium neodium iron intermediate alloy that will be prepared in the present embodiment takes praseodymium neodium iron intermediate alloy 8kg, with addition of iron staff as raw material
9kg, is smelted in 30kg intermediate frequency vaccum sensitive stoves, and protective gas is argon gas, and crucible selects praseodymium neodymium oxide crucible, after smelting
The praseodymium neodymium ferrous components for obtaining are shown in Table 14.
The praseodymium neodymium-iron alloy composition analysis result of table 14/wt%
| RE | Fe | C | O | P | S | Si | Mn |
| 40.05 | 59.77 | 0.0070 | 0.0086 | ＜ 0.01 | ＜ 0.005 | 0.0034 | ＜ 0.005 |
Term used herein is explanation and exemplary and nonrestrictive term.Because the present invention can be with various
Form specific implementation without deviating from invention it is spiritual or substantive, it should therefore be appreciated that above-described embodiment be not limited to it is any foregoing
Details, and widely being explained in the spirit and scope that should be limited in appended claims, thus fall into claim or its etc.
Whole changes and remodeling in the range of effect all should be appended claims and covered.
Claims (6)
1. a kind of praseodymium neodymium-iron alloy, it is characterised in that：The content of praseodymium neodymium is 0~95wt%, and surplus is that iron and total amount are less than
The inevitable impurity of 0.5wt%, wherein oxygen≤0.01wt%, carbon≤0.01wt%, phosphorus≤0.01wt%, sulphur≤
0.005wt%.
2. a kind of preparation method of praseodymium neodymium-iron alloy, including：
In the equipment of electrolysis praseodymium neodium iron intermediate alloy, under the fluoride molten salt electrolyte system of praseodymium fluoride neodymium and lithium fluoride,
It is electrolysis raw material with praseodymium neodymium oxide, is passed through direct current electrolysis and obtains praseodymium neodium iron intermediate alloy；
Using praseodymium neodium iron intermediate alloy and iron as raw material, convert method and prepare praseodymium neodymium-iron alloy using molten；In praseodymium neodymium-iron alloy, praseodymium neodymium
Content be 0~95wt%, surplus is the inevitable impurity of iron and total amount less than 0.5wt%, wherein oxygen≤
0.01wt%, carbon≤0.01wt%, phosphorus≤0.01wt%, sulphur≤0.005wt%.
3. the preparation method of praseodymium neodymium-iron alloy as claimed in claim 2, it is characterised in that：It is electrolysed the equipment of praseodymium neodium iron intermediate alloy
Electrolytic cell is done with graphite, graphite cake has the receiver for containing alloy as anode, iron staff as consumable negative electrode, negative electrode lower section.
4. the preparation method of praseodymium neodymium-iron alloy as claimed in claim 3, it is characterised in that：Praseodymium neodium iron intermediate alloy is molten to convert praseodymium neodymium iron
The equipment of alloy is intermediate frequency furnace, and molten to convert process and carry out under vacuum, crucible uses rare earth oxide crucible.
5. the preparation method of praseodymium neodymium-iron alloy as claimed in claim 3, it is characterised in that：Receiver material selection iron, rare earth oxygen
Compound or boron nitride.
6. the preparation method of praseodymium neodymium-iron alloy as claimed in claim 2, it is characterised in that：Also include gold during vacuum melts and converts
Category praseodymium neodymium or iron.
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| CN202110398830.4A CN113265684A (en) | 2016-12-16 | 2016-12-16 | Praseodymium neodymium iron alloy |
| CN202110398832.3A CN113279018B (en) | 2016-12-16 | 2016-12-16 | Use of praseodymium neodymium iron alloy in rare earth steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411372A (en) * | 2019-09-10 | 2020-07-14 | 包头稀土研究院 | Preparation method of rare earth iron alloy |
| CN113308633A (en) * | 2021-06-01 | 2021-08-27 | 包头市华星稀土科技有限责任公司 | Preparation method of praseodymium-neodymium alloy |
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| CN113279018B (en) | 2023-01-03 |
| CN113279018A (en) | 2021-08-20 |
| CN113265684A (en) | 2021-08-17 |
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