CN101591738B - Method for preparing magnesium-gadolinium-yttrocalcite ternary intermediate alloy - Google Patents
Method for preparing magnesium-gadolinium-yttrocalcite ternary intermediate alloy Download PDFInfo
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- CN101591738B CN101591738B CN2009100543204A CN200910054320A CN101591738B CN 101591738 B CN101591738 B CN 101591738B CN 2009100543204 A CN2009100543204 A CN 2009100543204A CN 200910054320 A CN200910054320 A CN 200910054320A CN 101591738 B CN101591738 B CN 101591738B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 97
- 239000000956 alloy Substances 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000007670 refining Methods 0.000 claims abstract description 35
- 238000003723 Smelting Methods 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000000155 melt Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 abstract description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052749 magnesium Inorganic materials 0.000 abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 11
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 230000008018 melting Effects 0.000 description 18
- 238000002844 melting Methods 0.000 description 18
- 229910052727 yttrium Inorganic materials 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- 238000005275 alloying Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 229910000946 Y alloy Inorganic materials 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 3
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- 230000001550 time effect Effects 0.000 description 1
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Abstract
The invention discloses a method for preparing a magnesium-gadolinium-yttrocalcite ternary intermediate alloy in the technical field of metallurgy, which comprises the following steps: preheating a Mg-Y binary intermediate alloy and a Mg-Gd binary intermediate alloy to 150 to 350 DEG C; putting the Mg-Y binary intermediate alloy in a smelting furnace for smelting and starting to introduce a protective gas when the temperature rises to 400 to 500 DEG C; after the Mg-Y binary intermediate alloy is smelted completely, rising the temperature to 730 to 750 DEG C, and adding the Mg-Gd binary intermediate alloy; after the Mg-Gd binary intermediate alloy is smelted completely, keeping the temperature of the melt between 730 to 750 DEG C, adding a refining agent, and refining the melt; and after the refining, keeping the temperature at 730 to 750 DEC C, and standing the melt to obtain the Mg-Gd-Y ternary intermediate alloy. The preparation method of the invention avoids the use of pure magnesium, saves time for smelting pure magnesium, reduces the oxidization and burning loss of magnesium elements in a pure magnesium smelting process, and achieves high rare earth element yield.
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 ウ system-heavily uncommon scholar Class mischmetal Forging property made お I 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-, 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)
1. the preparation method of a magnesium-gadolinium-yttrocalcite ternary master alloy is characterized in that, 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.
2. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, in the step 1, described Mg-Y binary master alloy is the Y of Mg and 5～10wt.%.
3. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, described Mg-Gd binary master alloy is the Gd of Mg and 60～80wt.%.
4. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, 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.
5. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, in the step 3, described adding is specially: clamping Mg-Gd binary master alloy places under the liquid level of liquation, mild agitation simultaneously.
6. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1, it is characterized in that in the step 4, the add-on of described refining agent is 1～4% of a liquation gross weight, before refining,, in refining process, evenly be sprinkling upon in the liquation and stirring to the refining agent preheating.
7. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, 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%.
8. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, in the step 4, described refining time is 5～12 minutes.
9. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, in the step 5, also will remove the scum silica frost of molten surface and the deposition slag of bottom after described refining is finished, and leaves standstill afterwards.
10. the preparation method of magnesium-gadolinium-yttrocalcite ternary master alloy according to claim 1 is characterized in that, in the step 5, described time of repose is 10～40 minutes.
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| 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 |
| CN103924107B (en) * | 2014-03-21 | 2016-06-22 | 南昌大学 | The preparation method of aluminum neodymium samarium ternary intermediate alloy |
| CN103924106B (en) * | 2014-03-21 | 2016-04-13 | 南昌大学 | The preparation method of aluminium praseodymium holmium ternary master alloy |
| CN104004931B (en) * | 2014-03-21 | 2016-06-15 | 南昌大学 | The preparation method of aluminum cerium yttrium ternary intermediate alloy |
| CN115161504A (en) * | 2022-08-03 | 2022-10-11 | 重庆大学 | Design method for preparing high-concentration high-performance magnesium alloy based on Mg-Gd-Y and magnesium alloy |
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