CN110373591A - A kind of magnetic material SmCo iron copper zirconium alloy and preparation method thereof - Google Patents
A kind of magnetic material SmCo iron copper zirconium alloy and preparation method thereof Download PDFInfo
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- CN110373591A CN110373591A CN201910705262.0A CN201910705262A CN110373591A CN 110373591 A CN110373591 A CN 110373591A CN 201910705262 A CN201910705262 A CN 201910705262A CN 110373591 A CN110373591 A CN 110373591A
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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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- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- 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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
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Abstract
The invention discloses a kind of magnetic material preparation method of SmCo iron copper zirconium alloy, alloying components are as follows: samarium 60~95wt% of content, cobalt content are 2~40wt%, surplus is iron, copper, zr element, wherein Fe≤2~40wt%, Cu≤1~7wt%, Zr≤1~6wt%.SmCo iron copper zirconium alloy is prepared using the method for fluoride molten salt electrolytic oxidation samarium.Cathode is made after molten alloy, ingot casting by the cobalt of corresponding purity, iron, copper and zirconium pure metal in cathode for electrolyzing.SmCo iron copper zirconium alloy prepared by this method has the advantages that stable components, uniform, impurity content is low etc., is the high-quality new raw material of one kind for preparing high-performance SmCo magnetic material.
Description
Technical field
The present invention relates to a kind of rare-earth alloy material, it is related to a kind of SmCo iron copper zirconium alloy and preparation method thereof.
Background technique
SmCo magnetic material is one kind using powder metallurgy process preparation with coercivity is big, Curie temperature is high, temperature
The more excellent rare earth permanent-magnetic material of the performances such as good, corrosion resistance of stability.Have become modern aerospace, defence and military, micro-
The indispensable important meals functional material in the fields such as wave device, communication, Medical Devices, motor.Market prospects are persistently become better.
Continuous improvement with SmCo magnetic material application field and the market demand to its performance and cost performance, prepares it
Higher requirements are also raised for technology and properties of product.In order to meet the needs of users, SmCo magnetic material technology of preparing is surrounded
More research work has been carried out in optimization and the promotion of preparation material quality.Used in existing SmCo magnetic materials production technology
Raw material after melting SmCo copper zirconium alloy, pass through system in vaccum sensitive stove using the single metal such as samarium, cobalt, iron, zirconium as raw material
The technical process such as powder, die mould, sintering prepare SmCo magnetic material.
Its technology of existing method prepares SmCo copper zirconium alloy and has the disadvantage that 1. existing samarium metal preparation processes
It is to be prepared by rare earth metal reduction-oxidation samarium, process flow is long, high expensive.2. samarium metal and cobalt, iron, copper, zirconium etc. are single
One metal differs greatly in basic physical properties such as fusing point, vapour pressure, density, and the fluctuation of institute's molten alloy ingredient and component segregation are existing
As obvious, the fluctuation of SmCo iron copper zirconium alloy ingredient is larger, generates large effect to prepared samarium-cobalt magnet consistency of performance.
3. causing this method to prepare since objectionable impurities elements oxygen content is relatively high (O > 0.2%) in the single metal such as metallic cobalt, zirconium
SmCo iron copper zirconium alloy in oxygen content it is higher, the samarium-cobalt magnet prepared with the alloy generates biggish negatively influencing to its performance.
Summary of the invention
Technical problem solved by the invention is to provide a kind of preparation method of magnetic material SmCo iron copper zirconium alloy, system
Standby SmCo iron copper zirconium alloy ingredient is uniform, stability is good, oxygen impurities content is low, rare-earth yield is high, using prepared by the present invention
SmCo iron copper zirconium alloy make raw material, prepare SmCo magnetic material and have a clear superiority in terms of its performance and stability,
And there is cost advantage.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of magnetic material SmCo iron copper zirconium alloy, by
The group of following weight percentage is grouped as:
Samarium 60~95%,
Cobalt 1~40%,
Surplus is iron, copper, zr element, and wherein weight percentage shared by Fe contains less than weight percent shared by 1~40%, Cu
Amount is less than weight percentage shared by 1~7%, Zr less than 1~6%.
Above-mentioned SmCo iron copper zirconium alloy is prepared using the method for fluoride molten salt electrolytic oxidation samarium.Electrolytic preparation SmCo iron copper
The electrolytic cell of zircaloy is the round electrolytic cell processed by graphite electrode, which also serves as anode, and cathode is the conjunction of ferro-cobalt copper zirconium
Alloy collector is arranged in the rodlike consumable cathode of gold, cathode lower section.Electrolyte is by samaric fluoride, lithium fluoride, barium fluoride in a cell
The molten salt electrolyte composition of mixed fluoride object composition.Electrolysis raw material is samarium oxide, is dissolved in by samaric fluoride, lithium fluoride, fluorine
In the molten-salt electrolysis plastidome for changing barium mixed fluoride object composition, logical direct current is electrolysed to obtain SmCo iron copper zirconium alloy.Electrolysis is with certainly
Consume cathode by the cobalt of corresponding purity, iron, copper and zirconium pure metal through vacuum high-temperature smelting furnace under low vacuum argon gas protective condition, melt
It is made after fusion aurification, ingot casting.Crucible for smelting material is magnesia crucible.
Compared with the prior art, the present invention has following technical advantage:
1, the present invention develop it is a kind of prepare SmCo magnetic material new SmCo iron copper zirconium alloy and its new preparation process, it is prepared
Copper zirconium alloy components Component it is stable, uniformly, alloy melting point it is lower.One is provided for the stable SmCo magnetic material of production performance
Kind raw material guarantee.
2, using SmCo iron copper zirconium alloy prepared by the present invention, influence prepares SmCo magnetic material performance in alloy
Critical impurities elemental oxygen content significantly reduces, and it is former to provide high-quality hypoxemia SmCo iron copper zirconium for preparation high-performance SmCo magnetic material
Material.
3, the rodlike consumable cathode of ferro-cobalt copper zirconium alloy is prepared using vacuum melting, cobalt, iron, copper, zirconium each element in alloy
Ingredient is accurately controllable.
4, SmCo iron copper zirconium alloy product of the present invention is using samarium oxide as raw material, compared with existing procedure, preparation flow
Short, cost and solid waste product are low, rare earth element high income.
5, product good market prospect.In recent years, with high-technology field for example new-energy automobile, rail traffic, robot,
The rise of the industries such as intelligence manufacture has in terms of being centered around high and low temperature and varying with temperature Magnetic stability and corrosion resistance
The SmCo magnetic material market demand speedup of superperformance is obvious.According to related market prediction, this growth trend will be in future
Longer term will persistently keep this growing trend, therefore SmCo magnetic material application wide market.
Detailed description of the invention
Attached drawing 1 is the structural schematic diagram that SmCo iron copper zirconium alloy electrolytic cell is electrolysed in the present invention.
Attached drawing 2 is SmCo iron copper zirconium alloy preparation technology flow chart in the present invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments:
Electrolysis SmCo iron copper zirconium alloy electrolysis unit used in the present invention is usually to be electrolysed dilute in fluoride salt electrolyte system
Native oxide prepares metal and alloy tests electrolysis unit used.It include: 1, electric heating furnace body, 2, graphitic cell (simultaneous sun
Pole), 3, ferro-cobalt copper zirconium alloy cathode, 4, alloy receipts collector.In use, graphitic cell is provided with electrolyte, electrolyte by
The molten salt electrolyte composition that samaric fluoride, lithium fluoride, barium fluoride mixed fluoride object form, cathode lower section are arranged alloy collector, receive
Collect the SmCo iron copper zirconium alloy of electrolytic preparation.The material of alloy collector can be one of aluminium oxide, magnesia.
The technology of preparing of SmCo ferrozirconium copper alloy is prepared, successively includes following procedure:
1, electrolytic cell is done with graphite, and doubles as anode, ferro-cobalt zirconium copper alloy is collected as consumable cathode, cathode lower section setting alloy
Device；Collector can be one of aluminium oxide, magnesia.
2, electrolyte is made of samaric fluoride, lithium fluoride, barium fluoride mixed fluoride object in a cell.Being electrolysed raw material is oxidation
Samarium is dissolved in the molten salt electrolyte being made of samaric fluoride, lithium fluoride, barium fluoride mixed fluoride object, leads to direct current electrolysis
Obtain SmCo iron copper zirconium alloy.
3, electrolysis with consumable cathode by the cobalt of corresponding purity, iron, copper and zirconium pure metal in a vacuum frequency induction melting furnace,
Using argon gas as protective gas, will be made after alloy molten alloying, ingot casting.Crucible for smelting material is magnesia crucible.
4, in prepared SmCo ferrozirconium copper alloy, alloying component are as follows: samarium 60~95wt% of content, cobalt content 1.5
~40wt%, surplus are iron, copper, zr element, wherein Fe≤1~40wt%, Cu≤1~7wt%, Zr≤1~6wt%.Surplus
It is the inevitable impurity that total amount is less than 0.3wt%, wherein oxygen≤0.015wt%, carbon≤0.015wt%, nitrogen≤
0.01wt%.
Embodiment 1
In the present embodiment the preparation of ferro-cobalt copper zirconium consumable cathode be using purity greater than 99.8% cobalt, iron, copper, zirconium pure metal as
Raw material carries out melting, melting according to the component ratio ingredient for standby consumable cathode ferro-cobalt copper zirconium of drawing up in intermediate frequency vaccum sensitive stove
For process using argon gas as protective gas, crucible is magnesia crucible, after metal molten, keeps the temperature 5 minutes, institute's melted alloy is poured into column
Ingot casting in shape ingot mould.The ferro-cobalt zirconium copper alloy ingot ingredient obtained after melting is shown in Table 1.The ingot is used as and prepares SmCo ferrozirconium copper alloy
Consumable cathode.
1 ferro-cobalt zirconium copper alloy composition analysis result (wt%) of table
| Element | Co | Fe | Cu | Zr | Si | Mn | Mg | O | C |
| Ingredient | 50 | 38 | 6 | 5.8 | 0.03 | 0.05 | 0.02 | 0.15 | 0.022 |
Using the circular graphitic electrolytic cell of the mm of Φ 120mm × 140, graphite cuvette doubles as anode, and samaric fluoride is in electrolyte
90wt%, lithium fluoride 10wt%, cathode are Φ 10mm ferro-cobalt zirconium alloy bar, average current intensity 120A, cathode-current density
5-8A/cm 2, 0.2/ A cm of anodic current density 2, electrolysis temperature is 1000 DEG C, is electrolysed 1 hour, samarium oxide additional amount is
SmCo ferrozirconium 113.5g is made in 123g, and samarium content is 89%, and alloying component the results are shown in Table 2.
2 SmCo ferrozirconium copper alloy composition analysis result (wt%) of table
| Element | Sm | Co | Fe | Cu | Zr | Mn | Mg | Si | O | C |
| Ingredient | 88.9 | 5.5 | 4.2 | 0.65 | 0.62 | 0.03 | 0.018 | 0.029 | 0.011 | 0.02 |
Embodiment 2
The preparation method of ferro-cobalt zirconium copper consumable cathode is same as Example 1 in the present embodiment.The preparation of ferro-cobalt copper zirconium consumable cathode
It is cobalt using purity greater than 99.8%, iron, copper, zirconium pure metal as raw material.According to the ingredient for standby consumable cathode ferro-cobalt copper zirconium of drawing up
Ratio ingredient, the ferro-cobalt copper zirconium alloy ingot ingredient obtained after melting are shown in Table 3.The ingot is as the consumable for preparing SmCo iron copper zirconium alloy
Cathode.
3 ferro-cobalt zirconium copper alloy composition analysis result (wt%) of table
| Element | Co | Fe | Cu | Zr | Mn | Mg | Si | O | C |
| Ingredient | 70 | 19 | 6 | 3.9 | 0.035 | 0.021 | 0.025 | 0.16 | 0.02 |
Using the circular graphitic electrolytic cell of the mm of Φ 120mm × 140, graphite cuvette doubles as anode, and samaric fluoride is in electrolyte
70wt%, lithium fluoride 30wt%, cathode are Φ 10mm ferro-cobalt zirconium alloy bar, average current intensity 120A, cathode-current density
8-10A/cm 2, anodic current density 0.5A/cm2, electrolysis temperature is 1050 DEG C, it is electrolysed 1 hour, samarium oxide additional amount 120g,
SmCo ferroalloy 101.5g is made, samarium content is 85%, and alloying component the results are shown in Table 4.
4 SmCo ferrozirconium composition analysis result (wt%) of table
| Element | Sm | Co | Fe | Cu | Zr | Mn | Mg | Si | O | C |
| Ingredient | 85 | 10.4 | 2.9 | 0.9 | 0.6 | 0.04 | 0.02 | 0.028. | 0.012 | 0.018 |
Embodiment 3
The preparation method of the polynary consumable cathode of ferro-cobalt zirconium is same as Example 1 in the present embodiment.The system of ferro-cobalt copper zirconium consumable cathode
Standby is cobalt using purity greater than 99.8%, iron, copper, zirconium pure metal as raw material.According to standby consumable cathode ferro-cobalt copper zirconium of drawing up at
Divide ratio ingredient, the ferro-cobalt copper zirconium alloy ingot ingredient obtained after melting is shown in Table 5.The ingot is as the consumable for preparing ferro-cobalt copper zirconium alloy
Cathode.
5 ferro-cobalt copper zirconium alloy composition analysis result (wt%) of table
| Element | Co | Fe | Cu | Zr | Si | Mn | Mg | O | C |
| Ingredient | 90 | 4.8 | 3 | 2 | 0.02 | 0.04 | 0.016 | 0.162 | 0.021 |
Using the circular graphitic electrolytic cell of the mm of Φ 120mm × 140, graphite cuvette doubles as anode, and samaric fluoride is in electrolyte
80wt%, lithium fluoride 20wt%, cathode are Φ 10mm ferro-cobalt copper zirconium alloy stick, and average current intensity 120A, cathode current is close
Spend 4-6A/cm2, anodic current density 0.9A/cm 2, electrolysis temperature is 1030 DEG C, it is electrolysed 1 hour, samarium oxide additional amount 123g,
SmCo iron copper zirconium alloy 99.8g is made, samarium content is 81%, and alloying component the results are shown in Table 6.
6 SmCo iron copper zirconium member alloy component analysis result (wt%) of table
| Element | Sm | Co | Fe | Cu | Zr | Mn | Mg | Si | O | C |
| Ingredient | 81 | 16.92 | 0.90 | 0.57 | 0.38 | 0.03 | 0.015 | 0.019 | 0.08 | 0.019 |
Embodiment 4
The preparation method of the polynary consumable cathode of ferro-cobalt zirconium is same as Example 1 in the present embodiment.The system of ferro-cobalt copper zirconium consumable cathode
Standby is cobalt using purity greater than 99.8%, iron, copper, zirconium pure metal as raw material.According to standby consumable cathode ferro-cobalt copper zirconium of drawing up at
Divide ratio ingredient, the ferro-cobalt copper zirconium alloy ingot ingredient obtained after melting is shown in Table 5.The ingot is as the consumable for preparing ferro-cobalt copper zirconium alloy
Cathode.
5 ferro-cobalt copper zirconium alloy composition analysis result (wt%) of table
| Element | Co | Fe | Cu | Zr | Si | Mn | Mg | O | C |
| Ingredient | 90 | 4.8 | 3 | 2 | 0.02 | 0.04 | 0.016 | 0.162 | 0.021 |
Using the circular graphitic electrolytic cell of the mm of Φ 120mm × 140, graphite cuvette doubles as anode, and samaric fluoride is in electrolyte
80wt%, lithium fluoride 15wt%, barium fluoride 5wt%, cathode are Φ 10mm ferro-cobalt copper zirconium alloy stick, average current intensity
130A, cathode-current density 9-11A/cm2, anodic current density 1.1A/cm 2, electrolysis temperature is 1050 DEG C, it is electrolysed 1 hour,
SmCo iron copper zirconium alloy 110.5g is made in samarium oxide additional amount 133g, and samarium content is 87%, and alloying component the results are shown in Table 6.
6 SmCo iron copper zirconium member alloy component analysis result (wt%) of table
| Element | Sm | Co | Fe | Cu | Zr | Mn | Mg | Si | O | C |
| Ingredient | 87 | 11.6 | 0.62 | 0.38 | 0.26 | 0.028 | 0.014 | 0.019 | 0.06 | 0.015 |
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art's energy
The solution contents of the present invention much of that are simultaneously implemented accordingly, and it is not intended to limit the scope of the present invention.It is all spiritual according to the present invention
Equivalent change or modification made by essence, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of magnetic material SmCo iron copper zirconium alloy, it is characterised in that: be grouped as by the group of following weight percentage:
Samarium 60~95%,
Cobalt 1~40%,
Surplus is iron, copper, zr element, and wherein weight percentage shared by Fe contains less than weight percent shared by 1~40%, Cu
Amount is less than weight percentage shared by 1~7%, Zr less than 1~6%.
2. a kind of preparation method of magnetic material SmCo iron copper zirconium alloy according to claim 1, it is characterised in that:
It is electrolysed in the electrolytic cell of SmCo iron copper zirconium alloy, using ferro-cobalt copper zirconium alloy as cathode, samarium oxide is electrolysis raw material, by the oxidation
Samarium is dissolved in the molten-salt electrolysis plastidome being made of samaric fluoride, lithium fluoride, barium fluoride mixed fluoride object, and logical direct current is electrolysed
To SmCo iron copper zirconium alloy.
3. preparation method according to claim 2, it is characterised in that: electrolysis SmCo iron copper zirconium alloy electrolytic cell is done with graphite
Electrolytic cell body, graphite tank also serve as anode, and ferro-cobalt copper zirconium alloy stick is collected as consumable cathode, cathode lower section setting alloy
Device.
4. preparation method according to claim 2, it is characterised in that: ferro-cobalt copper zirconium alloy stick cathode, by vacuum intermediate-frequency sense
Furnace is answered, under vacuum conditions, cobalt, iron, copper zirconium metal are made through melting, casting rod, melting crucible is magnesia crucible.
5. preparation method according to claim 2, it is characterised in that: alloy collector material selection iron, cobalt or carbonization
Boron.
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Application publication date: 20191025 |