CN114277406A - Preparation method of rare earth erbium-iron alloy and rare earth erbium-iron alloy - Google Patents
Preparation method of rare earth erbium-iron alloy and rare earth erbium-iron alloy Download PDFInfo
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Abstract
The invention relates to a preparation method of rare earth erbium-iron alloy and the rare earth erbium-iron alloy, wherein the method takes a graphite crucible as an electrolytic bath; the graphite sheet is an anode; a pure iron rod is used as a cathode; the iron crucible is a metal receiver; erbium oxide is used as a raw material; barium fluoride and sodium fluoride are used as binary system electrolyte, electrolysis is carried out at 1090-1110 ℃, the current is 4000-4500A, the voltage is 12-15V, and the method comprises the following steps: drying the electrolytic cell; adding a binary system electrolyte, after melting to a certain degree, placing an iron crucible in the center of the furnace bottom, placing a pure iron rod above the iron crucible, and starting electrolysis; adding erbium oxide, and adjusting the pure iron rod down in time; and after electrolyzing for a period of time, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy. In the prepared rare earth erbium-iron alloy, the mass fractions of iron and erbium are respectively 15.1-18.2% and 81.3-84.4%; the method has the advantages of low energy consumption, high productivity, small deviation and convenience for large-scale production.
Description
Technical Field
The invention relates to the technical field of rare earth erbium-iron alloy correlation, in particular to a preparation method of rare earth erbium-iron alloy and the rare earth erbium-iron alloy.
Background
The preparation method of the erbium-iron alloy mainly comprises two methods: a metal pair doping high-temperature mutual dissolution method and a fluoride vacuum calcium thermal reduction method.
The high-temperature mutual dissolution method firstly produces metal erbium, and then the metal erbium and pure iron are mutually dissolved at high temperature in a vacuum environment, and the method has the characteristic of simple production method. The erbium-iron alloy produced by the counter doping method has high impurity content, high production energy consumption and high cost, while metal erbium can be produced by an electrolytic method theoretically, but the condition for producing the metal erbium by the method becomes rigorous due to the fact that the electrolytic temperature is up to 1461 ℃, the production process becomes complex, and general production enterprises are difficult to implement production by the method.
Therefore, the fluoride vacuum calcium thermal reduction method is generally adopted in industry to produce metal erbium. The production of erbium-iron alloy by fluoride calcium thermal reduction method is a relatively mature production process, and metal calcium is used as raw material to produce erbium-iron alloy in vacuum environment by using erbium fluoride and iron. Because the vacuum reduction method is used for production, the production energy consumption is still higher, expensive vacuum reduction equipment, tungsten and molybdenum crucibles and the like are needed, the production cost is high, and the productivity is low.
Disclosure of Invention
The invention mainly aims to overcome the defects in the prior art and provides a preparation method of a rare earth erbium iron alloy and the rare earth erbium iron alloy, which are used for solving the problems in the prior art.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: the preparation method of the rare earth erbium iron alloy takes a graphite crucible as an electrolytic bath; the graphite sheet is an anode; a pure iron rod with the purity of more than 99 percent is used as a cathode; the iron crucible is a metal receiver; erbium oxide is used as a raw material; barium fluoride and sodium fluoride are binary system electrolytes, wherein the mass fraction of the sodium fluoride is 5-35%, and the mass fraction of the barium fluoride is 65-95%; the electrolysis is carried out within the temperature range of 1090-1110 ℃, the average current is controlled to be 4000-4500A, the average voltage is 12-15V, and the method specifically comprises the following steps:
s1: baking the electrolytic cell for 12-28 h by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolysis process, a small amount of erbium oxide is added for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 15-25 min;
s5: and electrolyzing for 60-80 min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
As a further aspect of the present invention, there is provided: the pure iron rod contains less than 0.05% of manganese and less than 0.02% of carbon, and is a round rod with the diameter of 30-120 mm.
As a further aspect of the present invention, there is provided: the pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 350-470 mm.
As a further aspect of the present invention, there is provided: the graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 370-480 mm.
As a further aspect of the present invention, there is provided: the binary system electrolyte comprises 5-25% of sodium fluoride and 75-95% of barium fluoride.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 15.1 to 18.2 percent of iron and 81.3 to 84.4 percent of erbium, and the total amount of the components is 99.5 percent.
Compared with the prior art, the invention has the beneficial effects that:
barium fluoride and sodium fluoride are adopted as binary system electrolyte to electrolyze the erbium-iron alloy, and different electrolytic temperatures and electrolyte compositions are controlled to obtain the erbium-iron alloy with different erbium contents, so that the gold slag is well separated, the product consistency is good, metal inclusions are less, the secondary refining process is reduced, the metal direct recovery rate is improved, and the energy consumption and the production cost can be greatly reduced; the method is easy to operate, high in productivity, convenient for large-scale production, clean and pollution-free in production process, stable and good in persistence.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the embodiment of the invention, a preparation method of rare earth erbium-iron alloy and the rare earth erbium-iron alloy are disclosed, wherein a graphite crucible is used as an electrolytic bath; the graphite sheet is an anode; a pure iron rod with the purity of more than 99 percent is used as a cathode; the iron crucible is a metal receiver; erbium oxide is used as a raw material; barium fluoride and sodium fluoride are binary system electrolytes, wherein the mass fraction of the sodium fluoride is 5-35%, and the mass fraction of the barium fluoride is 65-95%; the electrolysis is carried out within the temperature range of 1090-1110 ℃, the average current is controlled to be 4000-4500A, the average voltage is 12-15V, and the method specifically comprises the following steps:
s1: baking the electrolytic cell for 12-28 h by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolysis process, a small amount of erbium oxide is added for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 15-25 min;
s5: and electrolyzing for 60-80 min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
Preferably, in the preparation method of the rare earth erbium iron alloy, the pure iron rod has a manganese content of less than 0.05% and a carbon content of less than 0.02%, and is a round rod with a diameter of 30-120 mm.
Preferably, in the preparation method of the rare earth erbium iron alloy, the pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 350-470 mm.
Preferably, in the preparation method of the rare earth erbium iron alloy, the graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 370-480 mm.
Preferably, in the preparation method of the rare earth erbium iron alloy, the binary system electrolyte composed of the barium fluoride and the sodium fluoride is provided, wherein the mass fraction of the sodium fluoride is 5% -25%, and the mass fraction of the barium fluoride is 75% -95%.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 15.1 to 18.2 percent of iron and 81.3 to 84.4 percent of erbium, and the total amount of the components is 99.5 percent.
The first embodiment is as follows:
a550 mm circular graphite electrolytic cell is adopted, the electrolytic cell is placed in a small steel sleeve, graphite powder is filled around the electrolytic cell, an upper opening is sealed by refractory cement, a corundum gasket is installed, the small steel sleeve is placed in a steel furnace shell, insulating materials, refractory materials and heat-insulating materials are filled around the small steel sleeve, a cover plate is installed, and an anode consists of 4 graphite plates, and the method specifically comprises the following steps:
s1: baking the electrolytic bath for 12h by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolytic process, erbium oxide is added in a small amount for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 15 min;
s5: and (4) after electrolyzing for 60min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
The pure iron rod has a manganese content of less than 0.05% and a carbon content of less than 0.02%, and is a round rod with a diameter of 30 mm.
The pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 350 mm.
The graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 370 mm.
The electrolyte comprises a binary system electrolyte consisting of barium fluoride and sodium fluoride, wherein the mass fraction of the sodium fluoride is 5%, and the mass fraction of the barium fluoride is 95%.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 15.1 percent of iron and 84.4 percent of erbium, and the total amount of the components is 99.5 percent.
Example two
A600 mm circular graphite electrolytic cell is adopted, the electrolytic cell is placed in a small steel sleeve, graphite powder is filled around the electrolytic cell, an upper opening is sealed by refractory cement, a corundum gasket is installed, the small steel sleeve is placed in a steel furnace shell, insulating materials, refractory materials and heat-insulating materials are filled around the small steel sleeve, a cover plate is installed, and an anode consists of 4 graphite plates, and the method specifically comprises the following steps:
s1: baking the electrolytic bath for 16h by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolytic process, erbium oxide is added in a small amount for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 18 min;
s5: and after electrolysis for 65min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
The pure iron rod has a manganese content of less than 0.05% and a carbon content of less than 0.02%, and is a round rod with a diameter of 50 mm.
The pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 380 mm.
The graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 390 mm.
The electrolyte comprises a binary system electrolyte consisting of barium fluoride and sodium fluoride, wherein the mass fraction of the sodium fluoride is 10%, and the mass fraction of the barium fluoride is 90%.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 15.8 percent of iron and 83.7 percent of erbium, and the total amount of the components is 99.5 percent.
EXAMPLE III
A650 mm circular graphite electrolytic cell is adopted, the electrolytic cell is placed in a small steel sleeve, graphite powder is filled around the electrolytic cell, the upper opening is sealed by refractory cement, a corundum gasket is installed, the small steel sleeve is placed in a steel furnace shell, insulating materials, refractory materials and heat-insulating materials are filled around the small steel sleeve, a cover plate is installed, and an anode consists of 4 graphite plates, and the method specifically comprises the following steps:
s1: baking the electrolytic bath for 20 hours by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolytic process, erbium oxide is added in a small amount for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 20 min;
s5: and (4) after electrolysis for 70min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
The pure iron rod has a manganese content of less than 0.05% and a carbon content of less than 0.02%, and is a round rod with a diameter of 70 mm.
The pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 410 mm.
The graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 420 mm.
The electrolyte comprises a binary system electrolyte consisting of barium fluoride and sodium fluoride, wherein the mass fraction of the sodium fluoride is 15%, and the mass fraction of the barium fluoride is 85%.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 16.6 percent of iron and 82.9 percent of erbium, and the total amount of the components is 99.5 percent.
Example four
A700 mm circular graphite electrolytic cell is adopted, the electrolytic cell is placed in a small steel sleeve, graphite powder is filled around the electrolytic cell, the upper opening is sealed by refractory cement, a corundum gasket is installed, the small steel sleeve is placed in a steel furnace shell, insulating materials, refractory materials and heat-insulating materials are filled around the small steel sleeve, a cover plate is installed, and an anode consists of 4 graphite plates, and the method specifically comprises the following steps:
s1: baking the electrolytic bath for 24 hours by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolytic process, erbium oxide is added in a small amount for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 23 min;
s5: and after electrolyzing for 75min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
The pure iron rod has a manganese content of less than 0.05% and a carbon content of less than 0.02%, and is a round rod with a diameter of 100 mm.
The pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 440 mm.
The graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 450 mm.
The electrolyte comprises a binary system electrolyte consisting of barium fluoride and sodium fluoride, wherein the mass fraction of the sodium fluoride is 20%, and the mass fraction of the barium fluoride is 80%.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 17.4 percent of iron and 82.1 percent of erbium, and the total amount of the components is 99.5 percent.
EXAMPLE five
A750 mm circular graphite electrolytic cell is adopted, the electrolytic cell is placed in a small steel sleeve, graphite powder is filled around the electrolytic cell, the upper opening is sealed by refractory cement, a corundum gasket is installed, the small steel sleeve is placed in a steel furnace shell, insulating materials, refractory materials and heat-insulating materials are filled around the small steel sleeve, a cover plate is installed, and an anode consists of 4 graphite plates, and the method specifically comprises the following steps:
s1: baking the electrolytic bath for 28h by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolytic process, erbium oxide is added in a small amount for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 25 min;
s5: and (4) after electrolyzing for 80min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
The pure iron rod has a manganese content of less than 0.05% and a carbon content of less than 0.02%, and is a round rod with a diameter of 120 mm.
The pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 470 mm.
The graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 480 mm.
The electrolyte comprises a binary system electrolyte consisting of barium fluoride and sodium fluoride, wherein the mass fraction of the sodium fluoride is 25%, and the mass fraction of the barium fluoride is 75%.
In the rare earth erbium iron alloy prepared by the method, the mass fraction is as follows: 18.2 percent of iron and 81.3 percent of erbium, and the total amount of the components is 99.5 percent.
The above detailed description is specific to a possible embodiment of the present invention, but the embodiment is not intended to limit the scope of the present invention, and equivalent implementations or modifications without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (6)
1. A preparation method of rare earth erbium iron alloy is characterized by comprising the following steps: the method takes a graphite crucible as an electrolytic bath; the graphite sheet is an anode; a pure iron rod with the purity of more than 99 percent is used as a cathode; the iron crucible is a metal receiver; erbium oxide is used as a raw material; barium fluoride and sodium fluoride are binary system electrolytes, wherein the mass fraction of the sodium fluoride is 5-35%, and the mass fraction of the barium fluoride is 65-95%; the electrolysis is carried out within the temperature range of 1090-1110 ℃, the average current is controlled to be 4000-4500A, the average voltage is 12-15V, and the method specifically comprises the following steps:
s1: baking the electrolytic cell for 12-28 h by using an arc striking machine or a heating element, and drying the furnace body;
s2: the power of the arc striking machine is turned on to 48Kw, and binary system electrolyte consisting of barium fluoride and sodium fluoride is continuously added into the furnace;
s3: when the electrolyte is molten and reaches 10cm below the upper edge of the electrolytic cell, placing an iron crucible in the center of the bottom of the furnace, placing a pure iron rod above the iron crucible, and electrifying direct current to start electrolysis;
s4: in the electrolysis process, a small amount of erbium oxide is added for multiple times or continuously and uniformly, and the pure iron rod is adjusted downwards once every 15-25 min;
s5: and electrolyzing for 60-80 min, taking out the iron crucible, casting into ingots, cooling and demolding to obtain the erbium-iron alloy.
2. The method of producing a rare earth erbium iron alloy according to claim 1, characterized in that: the pure iron rod contains less than 0.05% of manganese and less than 0.02% of carbon, and is a round rod with the diameter of 30-120 mm.
3. The method of producing a rare earth erbium iron alloy according to claim 1, characterized in that: the pure iron rod is a round rod body formed by tightly welding three round rods, and the cathode downward insertion depth is 350-470 mm.
4. The method of producing a rare earth erbium iron alloy according to claim 1, characterized in that: the graphite sheet is turned up and down for reuse after being used for 50 hours, and the depth of downward insertion is 370-480 mm.
5. The method of producing a rare earth erbium iron alloy according to claim 1, characterized in that: the binary system electrolyte comprises 5-25% of sodium fluoride and 75-95% of barium fluoride.
6. An erbium iron alloy produced according to the method of any one of claims 1 to 5, characterized in that: the rare earth erbium iron alloy prepared by the method comprises the following components in percentage by mass: 15.1 to 18.2 percent of iron and 81.3 to 84.4 percent of erbium, and the total amount of the components is 99.5 percent.
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