CN114107709A - Terbium-iron alloy preparation method - Google Patents
Terbium-iron alloy preparation method Download PDFInfo
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- CN114107709A CN114107709A CN202210077010.XA CN202210077010A CN114107709A CN 114107709 A CN114107709 A CN 114107709A CN 202210077010 A CN202210077010 A CN 202210077010A CN 114107709 A CN114107709 A CN 114107709A
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- terbium
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- C—CHEMISTRY; METALLURGY
- 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
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a preparation method of terbium-iron alloy, which comprises the following specific steps: adding prepared raw materials of terbium fluoride powder, metal calcium particles, iron powder and NaCl powder into a mixing machine, and uniformly mixing; adding the mixture into a tungsten crucible of vacuum induction equipment, filling argon for argon washing after the vacuum degree is lower than 10Pa, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, starting heating for thermal reduction operation, then casting, cooling along with furnace equipment, taking out and separating slag to obtain metal after preliminary separation; and putting the primarily separated metal into a tungsten crucible of a vacuum induction device again, filling argon for argon washing after the vacuum degree is lower than 10Pa, then carrying out device leakage detection, filling protective gas argon after the leakage detection is qualified, carrying out refining and impurity removal, keeping the material for 20-30 minutes after the material is completely melted, and casting the material into a metal ingot after the impurity removal to obtain the terbium iron alloy. The invention improves the problems of high production cost, multiple working procedures and long period.
Description
Technical Field
The invention relates to the technical field of rare-earth ferroalloy preparation research, in particular to a preparation method of terbium ferroalloy.
Background
The rare earth iron alloy is a combination of rare earth elements and iron elements, the rare earth alloys have different applications and different rare earth element contents, wherein the terbium iron alloy is an important one of the rare earth iron alloys.
At present, the preparation method of the traditional terbium-iron alloy is roughly as follows: the method comprises preparing pure metal terbium by vacuum calcium thermal reduction method with rare earth fluoride, and then blending and co-melting with pure iron rod according to a certain proportion to obtain terbium-iron alloy with different terbium contents. The disadvantages of this preparation method are: high production cost, multiple working procedures, long period, expensive equipment, serious environmental pollution and the like.
Disclosure of Invention
The invention aims at overcoming the defects of the prior terbium-iron alloy preparation technology, and provides a preparation method of the terbium-iron alloy, which reduces the preparation procedures and changes the traditional terbium-iron preparation technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of terbium-iron alloy comprises the following specific steps:
s1 preparation of raw materials
The method comprises the following steps that raw materials to be prepared comprise terbium fluoride powder, metal calcium particles, iron powder and NaCl powder, the dosage of the terbium fluoride powder, the dosage of the metal calcium particles and the dosage of the iron powder are calculated according to the content proportion of two components in the terbium iron alloy to be prepared and the corresponding relation in a reduction reaction, and the calculation result of the dosage of the terbium fluoride powder, the calculation result of the dosage of the metal calcium particles and the calculation result of the dosage of the iron powder are obtained;
the actual usage amount of the terbium fluoride powder is consistent with the calculation result of the usage amount of the terbium fluoride powder, and the actual usage amount of the metal calcium particles is 1.25 times of the calculation result of the usage amount of the metal calcium particles; the actual dosage of the iron powder is consistent with the calculation result of the dosage of the iron powder; the actual dosage of the NaCl powder is 20 percent of the actual dosage of the metal calcium particles;
s2, mixing the raw materials
Adding terbium fluoride powder, metal calcium particles, iron powder and NaCl powder into a mixer, and uniformly mixing to obtain a mixed raw material;
s3, heating and reducing
Adding the mixed raw materials into a tungsten crucible of vacuum induction equipment, filling argon for argon washing after the vacuum degree is lower than 10Pa, wherein the argon washing frequency is not lower than one time, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, starting heating for thermal reduction operation, controlling the temperature at 1400-1500 ℃ in the thermal reduction operation process, preserving the heat for 5-10 minutes, then casting, cooling along with furnace equipment, taking out and separating slag to obtain metal after preliminary separation;
s4 refining and removing impurities
And putting the primarily separated metal into a tungsten crucible of vacuum induction equipment again, filling argon for argon washing after the vacuum degree is lower than 10Pa, wherein the argon washing frequency is not lower than one time, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, carrying out refining impurity removal, controlling the temperature at 1450 and 1550 ℃ in the refining impurity removal process, keeping the temperature for 20-30 minutes after the materials are completely melted, and casting the materials into metal ingots after the impurity removal to obtain the terbium ferroalloy.
Specifically, in step S3, the heat is preserved for 10 minutes during the thermal reduction operation, and then the cast product is cast and cooled by furnace equipment, and then the slag is taken out and separated to obtain the metal after the initial separation.
Specifically, in step S4, when refining and removing impurities, the material is kept for 30 minutes after being completely melted, and after removing impurities, the molten material is cast into metal ingots to obtain the terbium-iron alloy.
The invention has the beneficial effects that: according to the invention, quantitative iron powder, terbium fluoride and calcium particles are uniformly mixed and then put into a vacuum induction furnace for smelting, and the content of terbium is controlled by controlling the proportion of terbium fluoride and iron powder, so that compared with the traditional terbium iron preparation process, the problems of high production cost, multiple working procedures and long period are solved; the terbium-iron alloy is formed by two forms of terbium-iron mechanical alloy and terbium-iron intermetallic compound, and the terbium-iron alloy made by the method is stronger than the traditional terbium-iron mechanical alloy in physical and chemical properties.
Detailed Description
The invention will be further illustrated with reference to specific examples:
a preparation method of terbium-iron alloy comprises the following specific steps:
s1 preparation of raw materials
The method comprises the following steps that raw materials to be prepared comprise terbium fluoride powder, metal calcium particles, iron powder and NaCl powder, the dosage of the terbium fluoride powder, the dosage of the metal calcium particles and the dosage of the iron powder are calculated according to the content proportion of two components in the terbium iron alloy to be prepared and the corresponding relation in a reduction reaction, and the calculation result of the dosage of the terbium fluoride powder, the calculation result of the dosage of the metal calcium particles and the calculation result of the dosage of the iron powder are obtained;
the actual usage amount of the terbium fluoride powder is consistent with the calculation result of the usage amount of the terbium fluoride powder, and the actual usage amount of the metal calcium particles is 1.25 times of the calculation result of the usage amount of the metal calcium particles; the actual dosage of the iron powder is consistent with the calculation result of the dosage of the iron powder; the actual dosage of the NaCl powder is 20 percent of the actual dosage of the metal calcium particles;
s2, mixing the raw materials
Adding terbium fluoride powder, metal calcium particles, iron powder and NaCl powder into a mixer, and uniformly mixing to obtain a mixed raw material;
s3, heating and reducing
Adding the mixed raw materials into a tungsten crucible of vacuum induction equipment, filling argon for argon washing after the vacuum degree is lower than 10Pa, wherein the argon washing frequency is not lower than one time, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, starting heating for thermal reduction operation, controlling the temperature at 1400-1500 ℃ in the thermal reduction operation process, preserving the heat for 5-10 minutes, then casting, cooling along with furnace equipment, taking out and separating slag to obtain metal after preliminary separation;
s4 refining and removing impurities
And putting the primarily separated metal into a tungsten crucible of vacuum induction equipment again, filling argon for argon washing after the vacuum degree is lower than 10Pa, wherein the argon washing frequency is not lower than one time, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, carrying out refining impurity removal, controlling the temperature at 1450 and 1550 ℃ in the refining impurity removal process, keeping the temperature for 20-30 minutes after the materials are completely melted, and casting the materials into metal ingots after the impurity removal to obtain the terbium ferroalloy.
Specific example 1:
adding 2 kg of terbium fluoride powder, 1 kg of iron powder, 0.7 kg of metal calcium particles and 0.14 kg of NaCl powder into a mixer for uniform mixing, then placing the mixture into a tungsten crucible in vacuum induction equipment, vacuumizing to below 10Pa, then filling argon gas for argon washing, performing argon washing twice, then performing equipment leakage detection, heating to 1500 ℃ and preserving heat for 10 minutes under the protection of argon gas after the leakage detection is qualified, then casting, cooling along with furnace equipment, and taking out and separating slag to obtain metal after preliminary separation;
and putting the primarily separated metal into a tungsten crucible in vacuum induction equipment again, vacuumizing to below 10Pa, filling argon for argon washing twice, detecting the leakage of the equipment, refining and removing impurities under the protection of argon after the leakage detection is qualified, controlling the temperature at 1450 and 1550 ℃ in the refining and removing impurities process, keeping the temperature for 20 minutes after the materials are completely melted, and casting the materials into metal ingots after the impurities are removed to obtain the terbium ferroalloy.
The obtained 2.46 kg terbium-iron alloy contains Tb 58.9%, Fe 40.2%, Ca 0.011% and O0.15%.
Specific example 2:
adding 2 kg of terbium fluoride powder, 0.8 kg of iron powder, 0.7 kg of metal calcium particles and 0.14 kg of NaCl powder into a mixer for uniform mixing, then placing the mixture into a tungsten crucible in vacuum induction equipment, vacuumizing to below 10Pa, then filling argon for argon washing twice, then carrying out equipment leakage detection, heating to 1400 ℃ and 1500 ℃ under the protection of argon after the leakage detection is qualified, preserving heat for 5 minutes, then casting, cooling along with furnace equipment, taking out and separating slag to obtain metal after primary separation;
and putting the primarily separated metal into a tungsten crucible in vacuum induction equipment again, vacuumizing to below 10Pa, filling argon for argon washing twice, detecting the leakage of the equipment, refining and removing impurities under the protection of argon after the leakage detection is qualified, controlling the temperature at 1450 and 1550 ℃ in the refining and removing impurities process, keeping the temperature for 30 minutes after all the materials are melted, and casting the materials into metal ingots after the impurities are removed to obtain the terbium ferroalloy.
The resulting 2.25 kg terbium-iron alloy contains Tb 64.4%, Fe 35.1%, Ca 0.013% and O0.18%.
According to the invention, quantitative iron powder, terbium fluoride and calcium particles are uniformly mixed and then put into a vacuum induction furnace for smelting, and the content of terbium is controlled by controlling the proportion of terbium fluoride and iron powder, so that compared with the traditional terbium iron preparation process, the problems of high production cost, multiple working procedures and long period are solved; the terbium-iron alloy is formed by two forms of terbium-iron mechanical alloy and terbium-iron intermetallic compound, and the terbium-iron alloy made by the method is stronger than the traditional terbium-iron mechanical alloy in physical and chemical properties.
The present invention has been described in connection with the specific embodiments, and it is obvious that the specific implementation of the present invention is not limited by the above-mentioned manner, and it is within the protection scope of the present invention as long as various modifications are made by using the method concept and technical solution of the present invention, or the present invention is directly applied to other occasions without modification.
Claims (3)
1. A preparation method of terbium-iron alloy is characterized by comprising the following specific steps:
s1 preparation of raw materials
The method comprises the following steps that raw materials to be prepared comprise terbium fluoride powder, metal calcium particles, iron powder and NaCl powder, the dosage of the terbium fluoride powder, the dosage of the metal calcium particles and the dosage of the iron powder are calculated according to the content proportion of two components in the terbium iron alloy to be prepared and the corresponding relation in a reduction reaction, and the calculation result of the dosage of the terbium fluoride powder, the calculation result of the dosage of the metal calcium particles and the calculation result of the dosage of the iron powder are obtained;
the actual usage amount of the terbium fluoride powder is consistent with the calculation result of the usage amount of the terbium fluoride powder, and the actual usage amount of the metal calcium particles is 1.25 times of the calculation result of the usage amount of the metal calcium particles; the actual dosage of the iron powder is consistent with the calculation result of the dosage of the iron powder; the actual dosage of the NaCl powder is 20 percent of the actual dosage of the metal calcium particles;
s2, mixing the raw materials
Adding terbium fluoride powder, metal calcium particles, iron powder and NaCl powder into a mixer, and uniformly mixing to obtain a mixed raw material;
s3, heating and reducing
Adding the mixed raw materials into a tungsten crucible of vacuum induction equipment, filling argon for argon washing after the vacuum degree is lower than 10Pa, wherein the argon washing frequency is not lower than one time, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, starting heating for thermal reduction operation, controlling the temperature at 1400-1500 ℃ in the thermal reduction operation process, preserving the heat for 5-10 minutes, then casting, cooling along with furnace equipment, taking out and separating slag to obtain metal after preliminary separation;
s4 refining and removing impurities
And putting the primarily separated metal into a tungsten crucible of vacuum induction equipment again, filling argon for argon washing after the vacuum degree is lower than 10Pa, wherein the argon washing frequency is not lower than one time, then carrying out equipment leakage detection, filling protective gas argon after the leakage detection is qualified, carrying out refining impurity removal, controlling the temperature at 1450 and 1550 ℃ in the refining impurity removal process, keeping the temperature for 20-30 minutes after the materials are completely melted, and casting the materials into metal ingots after the impurity removal to obtain the terbium ferroalloy.
2. The method of claim 1, wherein in step S3, the thermal reduction is performed for 10 minutes, and then casting is performed, and after cooling with furnace equipment, the slag is removed and separated to obtain the primarily separated metal.
3. The method of any one of claims 1-2, wherein in step S4, the refining and the impurity removal are performed by keeping the material molten for 30 minutes, and the molten material is cast into metal ingot after the impurity removal to obtain the terbium iron alloy.
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| CN202210077010.XA CN114107709A (en) | 2022-01-24 | 2022-01-24 | Terbium-iron alloy preparation method |
| CN202210552653.5A CN114703387A (en) | 2022-01-24 | 2022-01-24 | Terbium-iron alloy preparation method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003089857A (en) * | 2001-09-19 | 2003-03-28 | Toshiba Corp | Negative magnetostrictive material and its manufacturing method |
| CN1743104A (en) * | 2004-08-31 | 2006-03-08 | 任英良 | Terbium-iron (Fe2Tb) alloy powder preparing method |
| CN106756446A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | The hypoxemia rare earth steel preparation method of Rare-earth Iron intermediate alloy |
| CN110117752A (en) * | 2019-06-24 | 2019-08-13 | 江西理工大学 | A method of preparing samarium ferroalloy |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332053C (en) * | 2004-11-11 | 2007-08-15 | 宁波科宁达工业有限公司 | Multiplex rare-earth ferroalloy (RERAFe#-[2]) powder and method for preparing same |
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- 2022-01-24 CN CN202210077010.XA patent/CN114107709A/en active Pending
- 2022-01-24 CN CN202210552653.5A patent/CN114703387A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003089857A (en) * | 2001-09-19 | 2003-03-28 | Toshiba Corp | Negative magnetostrictive material and its manufacturing method |
| CN1743104A (en) * | 2004-08-31 | 2006-03-08 | 任英良 | Terbium-iron (Fe2Tb) alloy powder preparing method |
| CN106756446A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | The hypoxemia rare earth steel preparation method of Rare-earth Iron intermediate alloy |
| CN110117752A (en) * | 2019-06-24 | 2019-08-13 | 江西理工大学 | A method of preparing samarium ferroalloy |
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