CN111364066A - Short-process preparation method of rare earth magnesium alloy - Google Patents
Short-process preparation method of rare earth magnesium alloy Download PDFInfo
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Abstract
The invention relates to a short-process preparation method of rare earth magnesium alloy, belonging to the field of magnesium alloy smelting metallurgy. The method takes rare earth oxide REO and MgO as raw materials to carry out electrolysis in electrolyte solution; and then adding pure magnesium into the molten liquid, melting, stirring, removing slag, filtering, purifying, cooling and solidifying to obtain the high-quality rare earth magnesium alloy ingot. Rare earth elements are added into the rare earth magnesium alloy, rare earth oxides and magnesium oxide are directly used as raw materials, an electrolysis process is added, a covering agent fluoride solvent which is required to be added in the rare earth magnesium alloy smelting process is used as an electrolyte, the electrolyte and pure magnesium are smelted together, and the rare earth magnesium alloy is obtained through filtration and deep purification treatment. The method shortens the production flow of the rare earth magnesium alloy containing Gd, Y and Nd elements, has uniform distribution of the rare earth elements of the ingot blank, small fluctuation, high yield and low production energy consumption, improves the quality of the rare earth magnesium alloy ingot casting, improves the production efficiency and reduces the raw material and production cost.
Description
Technical Field
The invention relates to a short-process preparation method of a rare earth magnesium alloy, in particular to a preparation method which can effectively shorten the production process of the rare earth magnesium alloy containing Gd, Y and Nd elements, improve the ingot casting quality and reduce the cost, and belongs to the field of magnesium alloy smelting metallurgy.
Background
The rare earth elements Gd, Y and Nd have obvious aging strengthening effect in the magnesium alloy, and on the basis, the rare earth magnesium alloys such as Mg-Gd-Y series, Mg-Gd-Y-Nd series and the like are researched and developed through component optimization design, have excellent room-temperature and high-temperature mechanical properties, and are widely applied in the field of aerospace. The traditional casting process of the rare earth magnesium alloy comprises the following steps: melting pure magnesium → adding rare earth elements → stirring → adding refining agent for refining → deslagging → filtering and purifying → cooling → solidifying. The rare earth elements are added mainly in two ways: one is to add pure rare earth into the magnesium melt and prepare alloy by alloying. The other is to add rare earth elements through Mg-RE intermediate alloy.
The above-described addition method has the following problems: 1) Mg-RE (Gd, Y and Nd) intermediate alloy can be prepared by electrolytic eutectoid, and pure Gd, Y and Nd rare earth metal is obtained by removing magnesium by vacuum distillation, see patent 200610075921. X. The obtained rare earth and the intermediate alloy are very expensive, so that the raw material cost of the rare earth magnesium alloy is high; 2) pure rare earth or rare earth-magnesium intermediate alloy is added into pure magnesium for melting, so that the rare earth-magnesium alloy is prepared, and the preparation method relates to secondary melting, and has long production flow and high production cost; 3) since the specific gravity of the rare earth element is larger than that of magnesium, the rare earth element can be settled by adding pure rare earth and Mg-RE intermediate alloy in the preparation process, so that the ingot blank is easy to element segregate, and the quality of a large-size cast ingot is difficult to control; 4) the melting point of the rare earth element is much higher than that of magnesium, and the melting temperature needs to be increased in the melting process, so that magnesium burning loss is caused. The reason is one of the factors that rare earth magnesium alloys such as Mg-Gd-Y series, Mg-Gd-Y-Nd series and the like are not widely applied in civil fields such as automobiles, rail transit and the like.
Disclosure of Invention
The invention aims to provide a preparation method which can effectively shorten the production process of rare earth magnesium alloy containing Gd, Y and Nd elements, improve the quality of cast ingots and reduce the cost. The preparation method can effectively shorten the production process of the rare earth magnesium alloy containing Gd, Y and Nd elements, reduce the raw material cost and the production cost, improve the ingot casting quality, and can expand the application field of the rare earth magnesium alloy.
One of the key measures adopted by the invention is to add an electrolysis process in the traditional production process of the rare earth magnesium alloy, and the added raw material is a mixed material of REO and MgO, thereby shortening the production process and reducing the raw material cost and the production cost of the rare earth magnesium alloy.
The second key measure adopted by the invention is to directly add pure magnesium into the electrolytic solution to prepare the rare earth magnesium alloy. There are two major benefits: on one hand, the melting temperature is not required to be increased for melting rare earth like the traditional addition mode, but the preparation temperature of the rare earth magnesium alloy is reduced, the burning loss of pure magnesium is reduced, and the energy consumption is reduced because the melting point of pure magnesium is low; on the other hand, the electrolyzed rare earth element exists in an ion form, and is added into the pure magnesium in the ion form, so that the rare earth element is more uniformly distributed in the cast ingot, the segregation is reduced, and the quality of the cast ingot is improved.
The short-process preparation method of the rare earth magnesium alloy is used for preparing rare earth magnesium alloys containing more than two elements of Gd, Y and Nd, such as Mg-Gd-Y series, Mg-Gd-Nd series, Mg-Y-Nd series and Mg-Gd-Y-Nd series magnesium alloys, can effectively shorten the production process of the rare earth magnesium alloys containing Gd, Y and Nd elements, improve the quality of cast ingots and reduce the cost.
According to the method, an electrolysis process is added in the traditional production process of the rare earth magnesium alloy, and the raw material is a mixed material of REO and MgO, so that the production flow is shortened, and the raw material cost and the production cost of the rare earth magnesium alloy are reduced; then, pure magnesium is directly added into the electrolytic solution to prepare the rare earth magnesium alloy.
A short-process preparation method of rare earth magnesium alloy comprises the following steps:
(1) rare earth oxides REO and MgO are used as raw materials to carry out electrolysis in electrolyte solution;
(2) adding pure magnesium into the molten liquid, melting, stirring, removing slag, filtering, purifying, cooling and solidifying to obtain the rare earth magnesium alloy ingot.
In the process of preparing the rare earth magnesium alloy containing Gd, Y and Nd elements, the adopted raw material is the mixed material of REO and MgO, so that the cost of the raw material is reduced. REO is Gd2O3、Y2O3And Nd2O3Two or three of them.
The raw materials REO and MgO are mixed according to the weight percentage:
Gd2O3：20％～40％，Y2O3：20％～40％，MgO：60％～20％；
Gd2O3：40％～60％，Nd2O3：10％～20％，MgO：50％～20％；
Y2O3：40％～60％，Nd2O3：10％～20％，MgO：50％～20％；
or Gd2O3：20％～35％，Y2O3：20％～35％，Nd2O3：10％～20％，MgO：50％～10％。
The electrolyte used in the smelting process is a protective solvent barium fluoride and a rare earth fluoride which are necessary to be added in the process of smelting the rare earth magnesium alloy, wherein BaF2The content is 20 wt.% to 40 w%, REF3The content is 80 w% -60 w%; REF3Of yttrium-rich rare earth fluorides, e.g. YF3。
In the method, the mass ratio of the raw materials (rare earth oxides REO and MgO) to the electrolyte is 1: 2-1: 4.
The method comprises the following specific steps:
(1) the smelting adopts a medium-frequency induction furnace, a stainless steel crucible is arranged in the furnace, heat-insulating asbestos felt is wrapped outside the crucible, electrolyte raw materials are added into the crucible, the power is adjusted, and the electrolyte is melted;
(2) adding a graphite anode plate, electrifying, then starting to add a mixed raw material of REO and MgO, then inserting a tungsten cathode into the molten liquid, electrifying the cathode by direct current, and starting an electrolysis process; stirring in the electrolysis process, and taking out the cathode and the anode after electrolysis;
(3) directly adding pure magnesium into the melt, stirring for many times after the pure magnesium is melted, and blowing argon into the melt;
(4) and cooling after purifying treatment and deep filtration to obtain the high-quality rare earth magnesium alloy ingot.
Preferably, the temperature of the molten metal is 760-900 ℃ in the electrolysis process.
Preferably, the tungsten cathode is inserted into the melt, and the distance between the tungsten cathode and the bottom of the crucible is 10-20 cm.
Preferably, the electrolysis time is 30 to 100 minutes.
Preferably, in the step (3), after adding pure magnesium, Mg-Zr intermediate alloy can be added to obtain Mg-Gd-Y-Zr series, Mg-Nd-Y-Zr series, Mg-Gd-Nd-Zr series and Mg-Gd-Y-Nd-Zr series rare earth magnesium alloy.
The method can effectively shorten the production process of the rare earth magnesium alloy containing Gd, Y and Nd elements, improve the quality of cast ingots and reduce the cost. Rare earth elements are added into the rare earth magnesium alloy, rare earth oxide and magnesium oxide are directly used as raw materials, an electrolysis process is added, a covering agent fluoride solvent which is required to be added in the rare earth magnesium alloy smelting process is used as electrolyte, the electrolyte and pure magnesium are smelted together, and the Mg-Gd-Y system, the Mg-Nd-Y system, the Mg-Gd-Nd system and the Mg-Gd-Y-Nd system rare earth magnesium alloy are obtained through filtration and deep purification treatment.
The method provided by the invention is used for smelting the rare earth magnesium alloy at low temperature, so that the burning loss of pure magnesium can be reduced, and the energy consumption is reduced. The rare earth elements are added into the pure magnesium in an ion form, so that the rare earth elements are more uniformly distributed in the cast ingot, the segregation is reduced, and the quality of the cast ingot is improved.
The residual fluoride can be used in the rare earth magnesium alloy, can play a role in removing molten liquid impurities, and can be added with little or no solvent before the steps of purification treatment and deep filtration.
The electrolytic process is added in the process of preparing the rare earth magnesium alloy, the preparation process of the rare earth magnesium alloy is shortened, the raw material cost and the production cost of the rare earth magnesium alloy are reduced, the rare earth elements are added into the magnesium alloy in an ion form and are stirred, so that the rare earth elements are more uniformly distributed in the cast ingot, the segregation is reduced, and the quality of the cast ingot is improved. The cast ingot has less segregation, high quality and low cost, is suitable for industrial production, can break the high-price barrier of the rare earth magnesium alloy, and has good effect on popularizing the application range of the rare earth magnesium alloy.
Detailed Description
The invention firstly adds an electrolysis process in the traditional production process of the rare earth magnesium alloy, and the added raw material is a mixed material of REO and MgO, thereby shortening the production flow and reducing the raw material cost and the production cost of the rare earth magnesium alloy; secondly, pure magnesium is directly added into the electrolytic solution to prepare the rare earth magnesium alloy. The method can effectively shorten the production process of the rare earth magnesium alloy containing Gd, Y and Nd elements, improve the quality of cast ingots and reduce the cost.
The preparation method comprises the following steps:
(1) the smelting uses a medium-frequency induction furnace, a stainless steel crucible is arranged in the furnace, heat-insulating asbestos felt is wrapped outside the crucible, electrolyte raw materials are added into the crucible, the power is adjusted, the electrolyte is melted, the temperature of the melt is raised to 760-900 ℃, and the melt is kept until the electrolysis process is finished; the electrolyte used in the smelting process is a protective solvent barium fluoride and rare earth fluoride, BaF, which must be added in the process of smelting rare earth magnesium alloy2:REF3The weight ratio is (20-40) to (80-60).
(2) Adding a graphite anode plate, electrifying, then starting to add a mixed raw material of REO and MgO, then inserting a tungsten cathode into the melt within a certain distance from the bottom of the crucible, wherein the distance from the tungsten cathode to the bottom of the crucible is 10-20cm, electrifying the cathode with direct current, and starting an electrolysis process. Stirring in the electrolysis process, and taking out the cathode and the anode after electrolyzing for a certain time; the raw material is a mixed material of REO and MgO, so that the cost of the raw material is reduced. REO is Gd respectively2O3、Y2O3、Nd2O3According to the requirement of the added elements, the MgO can be mixed with two or three of the components. The mixing proportion of the rare earth element raw materials is as follows: weight percent Gd2O3:Y2O3MgO (20 to 40), 20 to 40, and 60 to 20); weight percent Gd2O3:Nd2O3MgO (40-60), 10-20 and 50-20); weight percent Y2O3:Nd2O3MgO (40-60), 10-20 and 50-20); weight percent Gd2O3:Y2O3:Nd2O3:MgO＝(20～35):(20～35):(10～20):(50～10)。
(3) Directly adding pure magnesium into the melt, stirring for many times after the pure magnesium is melted, and blowing argon into the melt;
(4) and starting the conventional step of smelting the rare earth magnesium alloy, and cooling after purifying treatment and deep filtration to obtain the high-quality rare earth magnesium alloy ingot.
Example 1:
200kg of Mg-7Gd-5Y-1Nd-0.5Zr (wt.%) rare earth magnesium alloy is prepared, and the raw materials of the rare earth are mixed into Gd2O3:Y2O3:Nd2O335:25:10:30 MgO and BaF as electrolyte2:YF3And (3) adding 80kg of electrolyte into the crucible with the size of phi 340 × 1500mm, heating the crucible to be molten, heating the crucible to 860 ℃, adding the mixed raw materials, placing a graphite anode and electrifying, placing the graphite anode into a cathode, starting electrolysis, stirring once every ten minutes, opening the anode and the cathode after 80 minutes, cooling the temperature to 800 ℃, starting adding pure magnesium and an Mg-Zr intermediate alloy, stirring, filtering, purifying, and cooling to obtain the rare earth magnesium alloy cast ingot.
The rare earth elements of the cast ingot are uniformly distributed: the actual composition of the upper/lower part of the ingot was measured as (wt.%): gd: 6.92/6.90; y: 5.04/5.09; nd: 1/1, respectively; zr: 0.48/0.49; the actual yield of the cast ingot is 85 percent by calculation, and compared with the traditional rare earth magnesium alloy preparation process, the method has the advantages of high yield, short production flow, low temperature and short time.
Example 2:
200kg of Mg-7Gd-1Nd-0.5Zr (wt.%) rare earth magnesium alloy is prepared, and the raw materials of the rare earth are mixed into Gd2O3:Nd2O3:MgO＝60:10:30, the electrolyte is BaF2:YF330:70, the size of the crucible is phi 340 × 1500mm, 80kg of electrolyte is added into the crucible and heated to be molten, the temperature is raised to 860 ℃, the mixed raw material is added, the graphite anode is placed and electrified, the cathode is placed, electrolysis is started, the anode and the cathode are stirred once every ten minutes, after 60 minutes, the pure magnesium and the Mg-Zr intermediate alloy are started to be added, stirring, filtering and purifying treatment are carried out, and cooling is carried out to obtain the rare earth magnesium alloy cast ingot.
The rare earth elements of the cast ingot are uniformly distributed: the actual composition of the upper/lower part of the ingot was measured as (wt.%): gd: 7.08/7.1; nd: 0.94/0.96; zr: 0.43/0.46; the actual yield of the cast ingot is 88 percent by calculation, and compared with the traditional rare earth magnesium alloy preparation process, the method has the advantages of high yield, short production flow, low temperature and short time.
Example 3:
200kg of Mg-8Y-1Nd-0.5Zr (wt.%) rare earth magnesium alloy is prepared, and the raw materials of the rare earth are mixed into Y2O3：Nd2O3: MgO 55:10:35, and electrolyte BaF2:YF3The method comprises the steps of (40: 60), adding 80kg of electrolyte into a crucible with the size of phi 340 × 1500mm, heating the crucible to be molten, heating the crucible to 860 ℃, adding mixed raw materials, placing a graphite anode and electrifying, placing the graphite anode into a cathode, beginning electrolysis, stirring once every ten minutes, opening the anode and the cathode after 50 minutes, beginning to add pure magnesium and Mg-Zr intermediate alloy, stirring, filtering, purifying, and cooling to obtain the rare earth magnesium alloy cast ingot.
The rare earth elements of the cast ingot are uniformly distributed: the actual composition of the upper/lower part of the ingot was measured as (wt.%): y: 8.13/8.11; nd: 0.98/1; zr: 0.45/0.43; the actual yield of the cast ingot is 83 percent by calculation, and compared with the traditional rare earth magnesium alloy preparation process, the method has the advantages of high yield, short production flow, low temperature and short time.
The method shortens the production flow of the rare earth magnesium alloy containing Gd, Y and Nd elements, has uniform distribution of the rare earth elements of the ingot blank, small fluctuation, high yield and low production energy consumption, improves the quality of the rare earth magnesium alloy ingot casting, improves the production efficiency and reduces the raw material cost and the production cost.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.
Claims (10)
1. A short-process preparation method of rare earth magnesium alloy comprises the following steps:
(1) rare earth oxides REO and MgO are used as raw materials to carry out electrolysis in electrolyte solution;
(2) adding pure magnesium into the molten liquid, melting, stirring, removing slag, filtering, purifying, cooling and solidifying to obtain the rare earth magnesium alloy ingot.
2. The short-process preparation method of the rare earth magnesium alloy according to claim 1, characterized in that: the REO is Gd2O3、Y2O3And Nd2O3Two or three of them.
3. The short-process preparation method of the rare earth magnesium alloy according to claim 2, characterized in that: the mixing proportion of REO and MgO is as follows by weight percent:
Gd2O3：20％～40％，Y2O3：20％～40％，MgO：60％～20％；
Gd2O3：40％～60％，Nd2O3：10％～20％，MgO：50％～20％；
Y2O3：40％～60％，Nd2O3：10％～20％，MgO：50％～20％；
or Gd2O3：20％～35％，Y2O3：20％～35％，Nd2O3：10％～20％，MgO：50％～10％。
4. The short-process preparation method of the rare earth magnesium alloy according to claim 1, characterized in that: the electrolyte is a protective solvent barium fluoride and a rare earth fluoride added in the process of smelting the rare earth magnesium alloy, wherein BaF2The content is 20w percent to 40w percent, REF3The content is 80w percent to 60w percent, REF3Is YF3。
5. The short-process preparation method of the rare earth magnesium alloy according to claim 1, characterized in that: the mass ratio of the raw materials to the electrolyte is 1: 2-1: 4.
6. The short-run preparation method of a rare earth magnesium alloy according to any one of claims 1 to 5, characterized in that: the method comprises the following specific steps:
(1) the smelting adopts a medium-frequency induction furnace, a stainless steel crucible is arranged in the furnace, heat-insulating asbestos felt is wrapped outside the crucible, electrolyte raw materials are added into the crucible, the power is adjusted, and the electrolyte is melted;
(2) adding a graphite anode plate, electrifying, then starting to add a mixed raw material of REO and MgO, then inserting a tungsten cathode into the molten liquid, electrifying the cathode by direct current, and starting an electrolysis process; stirring in the electrolysis process, and taking out the cathode and the anode after electrolysis;
(3) directly adding pure magnesium into the melt, stirring for many times after the pure magnesium is melted, and blowing argon into the melt;
(4) and cooling after purifying treatment and deep filtration to obtain the high-quality rare earth magnesium alloy ingot.
7. The short-process preparation method of rare earth magnesium alloy according to claim 6, characterized in that: in the electrolysis process, the temperature of the molten liquid is 760-900 ℃.
8. The short-process preparation method of rare earth magnesium alloy according to claim 6, characterized in that: the distance between the tungsten cathode and the bottom of the crucible is 10-20 cm.
9. The short-process preparation method of rare earth magnesium alloy according to claim 6, characterized in that: the electrolysis time is 30-100 minutes.
10. The short-process preparation method of rare earth magnesium alloy according to claim 6, characterized in that: after the addition of pure magnesium, an Mg-Zr master alloy was also added.
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| CN116240416A (en) * | 2022-12-14 | 2023-06-09 | 上海航天精密机械研究所 | Low-foam low-smoke refining agent for rare earth magnesium alloy and preparation method thereof |
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| 郭探 等: ""熔盐电解法制备稀土合金研究进展"", 《中国科学:化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116240416A (en) * | 2022-12-14 | 2023-06-09 | 上海航天精密机械研究所 | Low-foam low-smoke refining agent for rare earth magnesium alloy and preparation method thereof |
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