CN101591738A - Preparation method of magnesium gadolinium yttrium ternary master alloy - Google Patents
Preparation method of magnesium gadolinium yttrium ternary master alloy Download PDFInfo
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- CN101591738A CN101591738A CNA2009100543204A CN200910054320A CN101591738A CN 101591738 A CN101591738 A CN 101591738A CN A2009100543204 A CNA2009100543204 A CN A2009100543204A CN 200910054320 A CN200910054320 A CN 200910054320A CN 101591738 A CN101591738 A CN 101591738A
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- 239000000956 alloy Substances 0.000 title claims abstract 29
- 229910045601 alloy Inorganic materials 0.000 title claims abstract 29
- VLQDOBLEGJTQBO-UHFFFAOYSA-N [Y].[Gd].[Mg] Chemical compound [Y].[Gd].[Mg] VLQDOBLEGJTQBO-UHFFFAOYSA-N 0.000 title claims abstract 12
- 238000002360 preparation method Methods 0.000 title claims abstract 3
- 238000000034 method Methods 0.000 claims abstract 12
- 238000007670 refining Methods 0.000 claims abstract 11
- 239000000155 melt Substances 0.000 claims abstract 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract 5
- 238000003723 Smelting Methods 0.000 claims abstract 3
- 230000001681 protective effect Effects 0.000 claims abstract 3
- 238000002844 melting Methods 0.000 claims abstract 2
- 230000008018 melting Effects 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 2
- 239000011261 inert gas Substances 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims 1
- 229910001627 beryllium chloride Inorganic materials 0.000 claims 1
- LWBPNIJBHRISSS-UHFFFAOYSA-L beryllium dichloride Chemical compound Cl[Be]Cl LWBPNIJBHRISSS-UHFFFAOYSA-L 0.000 claims 1
- 239000001110 calcium chloride Substances 0.000 claims 1
- 229910001628 calcium chloride Inorganic materials 0.000 claims 1
- 235000011148 calcium chloride Nutrition 0.000 claims 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims 1
- 229910001634 calcium fluoride Inorganic materials 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000002893 slag Substances 0.000 claims 1
- 239000011780 sodium chloride Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract 4
- 229910052749 magnesium Inorganic materials 0.000 abstract 4
- 239000011777 magnesium Substances 0.000 abstract 4
- 238000005516 engineering process Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
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Abstract
一种冶金技术领域的镁钆钇三元中间合金的制备方法，包括如下步骤：预热Mg－Y二元中间合金和Mg－Gd二元中间合金到150～350℃；将Mg－Y二元中间合金加入到熔炼炉中，熔化，当温度升高到400～500℃时开始通入保护气体；当Mg－Y二元中间合金全部熔化后，升高温度到730～750℃，加入Mg－Gd二元中间合金；在Mg－Gd二元中间合金完全熔化后，将熔液的温度保持在730～750℃，加入精炼剂，精炼；精炼完成后，将温度保持在730～750℃静置，得到Mg－Gd－Y三元中间合金。本发明的制备方法没有使用纯镁，省去了熔炼纯镁的时间，减少了熔炼纯镁过程中镁元素的氧化和烧损，稀土元素的收得率高。
A method for preparing a magnesium-gadolinium-yttrium ternary master alloy in the field of metallurgy technology, comprising the following steps: preheating the Mg-Y binary master alloy and the Mg-Gd binary master alloy to 150-350°C; The master alloy is added to the melting furnace and melted. When the temperature rises to 400-500°C, the protective gas is introduced; when the Mg-Y binary master alloy is completely melted, the temperature is raised to 730-750°C, and Mg- Gd binary master alloy; after the Mg-Gd binary master alloy is completely melted, keep the temperature of the melt at 730-750°C, add refining agent, and refine; after refining, keep the temperature at 730-750°C and let stand , to get Mg-Gd-Y ternary master alloy. The preparation method of the invention does not use pure magnesium, saves the time for smelting pure magnesium, reduces the oxidation and burning loss of magnesium elements in the process of smelting pure magnesium, and has a high yield of rare earth elements.
Description
Technical field
The present invention relates to a kind of preparation method of metallurgical technology field, specifically is a kind of preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy.
Background technology
Development along with magnesium alloy, the Mg-RE series magnesium alloy with excellent mechanical property and high-temperature creep resistance in aerospace, military project, high-tech areas such as automobile have vast potential for future development, when the rapid expansion of kind of Mg-RE series magnesium alloy also correspondingly is applied in the industrial production, smelting technique to its magnesium-rare earth alloy has proposed new requirement: under the prerequisite that guarantees alloy property, in the shortest time, melt out qualified magnesium-rare earth alloy with minimum energy, the time of alloy melting and the loss of metallic element had both been reduced, save production cost, can accurately control the composition of alloy again.Thereby enhance productivity effectively, reduce and pollute.Therefore the simple method of finding out a kind of Mg-Gd-Y of preparation ternary master alloy is significant.
Consult document and find that traditional melting method of Mg-Gd-Y ternary master alloy mainly contains two kinds, (Gu Chimao is great for a kind of method of the used melting in research magnesium-rare earth alloy process that is the Japanese, the north mouth is rich; the Sickle scholar is heavy fine; little Island Yang; Seki Yi Zuofu, the Kubo Tagayasu Den is flat, the マ グ ネ シ ゥ system-heavily uncommon scholar Class mischmetal Forging property made ぉ ょ び Forging makes material Time effect characteristic と and draws the Zhang characteristic. light metal, 1997,47 (5): 261～266): its method is that to utilize purity be that 99.9% magnesium, pure rare earth Gd and pure rare earth Y are as raw material melting Mg-Gd-Y ternary master alloy.This method is to the equipment requirements height, the raw material costliness, and single furnace output is few, and the temperature of melting too high (830～870 ℃) is brought certain danger to production.The method of disclosed a kind of melting Mg-Gd-Y ternary master alloy is in patent CN 1676646A: earlier pure magnesium is put into smelting furnace and melt; the Mg-Gd master alloy is directly joined in the pure magnesium liquid then; when the Mg-Gd master alloy melts and melt temperature adds the Mg-Y master alloy when being elevated to 720～740 ℃ fully; and in this process, need constantly to pass to shielding gas or add insulating covering agent; owing to need the pure magnesium of melting; then the time of melting longer, the oxidation and the scaling loss of element are serious.Master alloy is because density is big, when melting, sink to the bottom fusing of liquation, simultaneously because the density of rare earth element is big, spread coefficient in the magnesium alloy liquation is little, rare earth element after the fusing is trapped in the bottom of melt, it is lower to cause alloying constituent to be difficult to the recovery rate controlled with raw material, is easy to generate sedimentation and component segregation, has seriously reduced working efficiency and has increased production cost.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy is provided.Preparation method of the present invention does not use pure magnesium, has saved the time of the pure magnesium of melting, has reduced the oxidation and the scaling loss of magnesium elements in the pure magnesium process of melting, the recovery rate height of rare earth element.
The present invention is achieved through the following technical solutions, and comprises the steps:
Step 1, preheating Mg-Y binary master alloy and Mg-Gd binary master alloy to 150～350 ℃;
Step 2 joins Mg-Y binary master alloy in the smelting furnace, and fusing begins to feed shielding gas when temperature is elevated to 400～500 ℃;
Step 3, when Mg-Y binary master alloy all after the fusing, elevated temperature to 730～750 ℃ add Mg-Gd binary master alloy;
Step 4 after Mg-Gd binary master alloy melts fully, remains on 730～750 ℃ with the temperature of liquation, adds refining agent, refining;
Step 5 after refining is finished, remains on 730～750 ℃ with temperature and leaves standstill, and obtains Mg-Gd-Y ternary master alloy.
In the step 1, described Mg-Y binary master alloy is Mg-(5～10wt.%) Y; Described Mg-Gd binary master alloy is Mg-(60～80wt.%) Gd.
In the step 2, described shielding gas is rare gas element, rare gas element and SF
6Gas mixture or CO
2With SF
6Gas mixture in a kind of.
In the step 3, described adding is specially: clamping Mg-Gd binary master alloy places under the liquid level of liquation, mild agitation simultaneously.
In the step 4, the add-on of described refining agent is 1～4% of a liquation gross weight, to the refining agent preheating, evenly is sprinkling upon in the liquation in refining process and stirring before refining.
In the step 4, the component of described refining agent and weight percent are: MgCl
240～50%, KCl 20～25%, CaF
210～15%, NaCl 10～15%, CaCl
23～5%, BeCl
23～5%.
In the step 4, described refining time is 5～12 minutes.
In the step 5, also to remove the scum silica frost of molten surface and the deposition slag of bottom after described refining is finished, leave standstill afterwards.
In the step 5, described time of repose is 10～40 minutes.
Compared with prior art, the present invention has following beneficial effect: preparation method of the present invention does not use pure magnesium, has saved the time of the pure magnesium of melting, has reduced the oxidation and the scaling loss of magnesium elements in the pure magnesium process of melting, the recovery rate height of rare earth element; Simultaneously, when in preparation process, using Mg-Gd binary master alloy dilution Mg-Y binary master alloy liquation, under Mg-Gd binary intermediate alloy ingot immersed in liquid level, and mild agitation, reduce the scaling loss of element, can quicken the diffusion of rare earth element simultaneously, promote the homogenizing of liquation composition.Melted magnesium-gadolinium-yttrocalcite ternary alloy also can be used as the finished product alloy and uses except using as master alloy.
Description of drawings
Fig. 1 is the as-cast structure pattern of embodiment 1;
Fig. 2 is the as-cast structure pattern of embodiment 2;
Fig. 3 is the as-cast structure pattern of embodiment 3.
Embodiment
Following example will the invention will be further described in conjunction with the accompanying drawings.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
The melting method of the Mg-Gd-Y ternary master alloy of 46kg, wherein alloying constituent (weight percent) is 11.83%Gd, 6.48%Y, all the other are Mg.
Step 1, getting its raw material is the Mg-10wt.%Y binary intermediate alloy ingot of 37.52kg and the Mg-60wt.%Gd binary intermediate alloy ingot of 10.34kg; The surface-conditioning of two kinds of binary master alloys is clean, and be preheating to 150 ℃;
Step 2 is opened smelting furnace, and its smelting furnace adopts the resistance melting furnace apparatus, and the Mg-10wt.%Y binary intermediate alloy ingot of 37.52kg is joined in the smelting furnace, and fusing heats up; When being elevated to 400 ℃, temperature begins to feed rare gas element Ar gas, anti-oxidation of protection liquation and burning;
Step 3, when Mg-Y binary master alloy all after the fusing, elevated temperature to 730 ℃ adds Mg-Gd binary master alloy; Original Mg-Y alloy liquation is diluted; Utilize cramp iron to clamp under the liquid level that the Mg-60wt.%Gd intermediate alloy ingot places liquation, and the mild agitation alloy pig, be beneficial to the acceleration of all even Elements Diffusion of composition;
Step 4 after Mg-Gd binary intermediate alloy ingot melts fully, remains on 730 ℃ with the temperature of liquation, and adding weight is the refining agent of liquation gross weight 1%, refining 7 minutes; The component of described refining agent and weight percent are: MgCl
250%, KCl 20%, CaF
210%, NaCl 10%, CaCl
25%, BeCl
25%;
Step 5 after refining is finished, is removed the scum silica frost on surface and the deposition slag of bottom, and temperature-stable at 730 ℃ and left standstill 35 minutes, is obtained Mg-Gd-Y ternary master alloy; Mg-Gd-Y ternary master alloy is poured into from smelting furnace in the metallicity mould of abundant preheating and is frozen into ingot casting.
Embodiment 2
The melting method of the Mg-Gd-Y ternary master alloy of 68kg, wherein alloying constituent (weight percent) is 7.88%Gd, 5.25%Y, all the other are Mg.
Step 1, getting raw material is the Mg-60wt.%Gd binary intermediate alloy ingot of Mg-7.5wt.%Y binary master alloy and the 10.2kg of 60.4kg; The surface-conditioning of two kinds of binary master alloys is clean, and be preheating to 250 ℃;
Step 2 is opened smelting furnace, and its smelting furnace adopts the resistance melting furnace apparatus, and just Mg-7.5wt.%Y binary intermediate alloy ingot joins in the smelting furnace, and fusing heats up; When being elevated to 450 ℃, temperature begins to feed Ar gas and SF
6Gas mixture, anti-oxidation of protection liquation and burning;
Step 3, when the alloy in the smelting furnace all after the fusing, elevated temperature to 740 ℃ adds Mg-60wt.%Gd binary intermediate alloy ingot; Original Mg-Y alloy liquation is diluted; Utilize cramp iron to clamp under the liquid level that the Mg-60wt.%Gd intermediate alloy ingot places liquation, and the mild agitation alloy pig, be beneficial to the acceleration of all even Elements Diffusion of composition;
Step 4 after Mg-Gd binary intermediate alloy ingot melts fully, remains on 740 ℃ with the temperature of liquation, and adding weight is the refining agent of liquation gross weight 2.5%, refining 10 minutes; The component of described refining agent and weight percent are: MgCl
240%, KCl 24%, CaF
215%, NaCl 15%, CaCl
23%, BeCl
23%;
Step 5 after refining is finished, is removed the scum silica frost on surface and the deposition slag of bottom, and temperature-stable at 740 ℃ and left standstill 25 minutes, is obtained Mg-Gd-Y ternary master alloy; Mg-Gd-Y ternary master alloy is poured into from smelting furnace in the metallicity mould of abundant preheating and is frozen into ingot casting.
Embodiment 3
The melting method of the Mg-Gd-Y ternary master alloy of 69kg, wherein alloying constituent (weight percent) is 10.5%Gd, 3.5%Y, all the other are Mg.
Step 1, getting raw material is the Mg-80wt.%Gd binary intermediate alloy ingot of Mg-5wt.%Y binary master alloy and the 10.4kg of 60.5kg; The surface-conditioning of two kinds of binary master alloys is clean, and be preheating to 350 ℃;
Step 2 is opened smelting furnace, and Mg-5wt.%Y binary master alloy is joined in the smelting furnace, and fusing heats up; When being elevated to 500 ℃, temperature begins to feed CO
2With SF
6Gas mixture, anti-oxidation of protection liquation and burning;
Step 3, when the alloy in the smelting furnace all after the fusing, elevated temperature to 750 ℃ adds Mg-80wt.%Gd binary intermediate alloy ingot, and original Mg-Y alloy liquation is diluted.Utilize iron clamp to fix the Mg-80wt.%Gd intermediate alloy ingot and place under the liquid level of liquation, and the mild agitation alloy pig, be beneficial to the acceleration of all even Elements Diffusion of composition;
Step 4 after Mg-Gd binary intermediate alloy ingot melts fully, remains on 750 ℃ with the temperature of liquation, and adding weight is the refining agent of liquation gross weight 4%, refining 11 minutes; The component of described refining agent and weight percent are: MgCl
245%, KCl 20%, CaF
215%, NaCl 12%, CaCl
24%, BeCl
24%;
Step 5 after refining is finished, is removed the scum silica frost on surface and the deposition slag of bottom, and temperature-stable at 750 ℃ and left standstill 15 minutes, is obtained Mg-Gd-Y ternary master alloy; Mg-Gd-Y ternary master alloy is poured into from smelting furnace in the metallicity mould of abundant preheating and is frozen into ingot casting.
Claims (10)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102312144A (en) * | 2010-07-07 | 2012-01-11 | 乐普（北京）医疗器械股份有限公司 | Ultrafine-grain medical magnesium alloy and preparation method thereof |
| CN103924107A (en) * | 2014-03-21 | 2014-07-16 | 南昌大学 | Preparation method of aluminum neodymium samarium ternary intermediate alloy |
| CN103924106A (en) * | 2014-03-21 | 2014-07-16 | 南昌大学 | Preparation method of aluminum praseodymium holmium ternary intermediate alloy |
| CN104004931A (en) * | 2014-03-21 | 2014-08-27 | 南昌大学 | Preparation method of ternary master alloy of aluminum, cerium and yttrium |
| CN115161504A (en) * | 2022-08-03 | 2022-10-11 | 重庆大学 | A design method and magnesium alloy for preparing high-concentration and high-performance magnesium alloy based on Mg-Gd-Y |
| CN119040676A (en) * | 2024-10-31 | 2024-11-29 | 赣州有色冶金研究所有限公司 | Preparation method of magnesium-containing yttrium-containing alloy |
-
2009
- 2009-07-02 CN CN2009100543204A patent/CN101591738B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102312144A (en) * | 2010-07-07 | 2012-01-11 | 乐普（北京）医疗器械股份有限公司 | Ultrafine-grain medical magnesium alloy and preparation method thereof |
| CN103924107A (en) * | 2014-03-21 | 2014-07-16 | 南昌大学 | Preparation method of aluminum neodymium samarium ternary intermediate alloy |
| CN103924106A (en) * | 2014-03-21 | 2014-07-16 | 南昌大学 | Preparation method of aluminum praseodymium holmium ternary intermediate alloy |
| CN104004931A (en) * | 2014-03-21 | 2014-08-27 | 南昌大学 | Preparation method of ternary master alloy of aluminum, cerium and yttrium |
| CN103924107B (en) * | 2014-03-21 | 2016-06-22 | 南昌大学 | The preparation method of aluminum neodymium samarium ternary intermediate alloy |
| CN115161504A (en) * | 2022-08-03 | 2022-10-11 | 重庆大学 | A design method and magnesium alloy for preparing high-concentration and high-performance magnesium alloy based on Mg-Gd-Y |
| CN119040676A (en) * | 2024-10-31 | 2024-11-29 | 赣州有色冶金研究所有限公司 | Preparation method of magnesium-containing yttrium-containing alloy |
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| CN101591738B (en) | 2010-10-06 |
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