CN108048718B - The production method of Mg-Zr intermediate alloy - Google Patents
The production method of Mg-Zr intermediate alloy Download PDFInfo
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- CN108048718B CN108048718B CN201710994951.9A CN201710994951A CN108048718B CN 108048718 B CN108048718 B CN 108048718B CN 201710994951 A CN201710994951 A CN 201710994951A CN 108048718 B CN108048718 B CN 108048718B
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- intermediate alloy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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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
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
Abstract
The invention discloses a kind of production method of Mg-Zr intermediate alloy, include the following steps: to melt magnesium metal in reacting furnace, and be passed through by CO2And SF6The mixed gas of composition, when reacting furnace temperature reaches 750~900 DEG C, low whipping speed is under the stirring action of 300~800r/min, and zirconium chloride is added in substep, reaction 1~2 hour after the completion of being added；Wherein, the SF in mixed gas6Percent by volume be 0.5vol%~1.5vol%, and the weight ratio of magnesium metal and zirconium chloride be 1:0.1~0.5.Production method of the invention can improve the zirconium distributing homogeneity in Mg-Zr intermediate alloy.
Description
Technical field
The present invention relates to a kind of production methods of Mg-Zr intermediate alloy.
Background technique
Magnesium alloy usually requires that some alloy elements are added to improve its performance.For example, magnesium conjunction can be improved in Al and Zn
The room temperature intensity of gold；The corrosion resisting property of magnesium alloy can be improved in Mn, Fe and other heavy metal elements；Magnesium can be improved in rare earth element
The recrystallization temperature of alloy, and slow down recrystallization process, to greatly improve the elevated temperature strength and creep-resistant property of magnesium alloy.Zr
Close-packed hexagonal lattice is belonged to Mg, and lattice constant is very close.Zr readily becomes nucleus when crystallization, hence it is evident that refinement is closed
Jin Jing's grain, to greatly improve the mechanical property of magnesium alloy.In addition, Zr to improve magnesium alloy corrosion resistance and heat resistance also have compared with
Big effect.
Zr in magnesium alloy is usually to be added in the form of Mg-Zr intermediate alloy.The intermediate alloy often restores zirconium fluorine with Mg
The method of sour potassium produces.For example, using KCl for solvent, magnesium metal, and the K with melting are melted at high temperature2ZrF6Reaction 5~
Then 10min is crushed, is washed, removal salt is mingled with, and Mg-Zr intermediate alloy is made in remelting.Due to salt impurity and alloy
Similar density, though removing the gred through washing, Zr distribution is very uneven in alloy obtained, to influence Mg-Zr intermediate alloy
It uses.
On the one hand, magnesium alloy can obtain with the following method: (1) will close among pure magnesium, 30.47%Gd magnesium gadolinium
Gold, 31.72%Y magnesium yttrium intermediate alloy and 30.16%Zr Mg-Zr intermediate alloy are melted at 730~750 DEG C, using CO2+SF6Mixing
Gas shield, casting, through 530 DEG C of homogenizing annealings for 24 hours after up to (referring to CN105525176A)；(2) by pure magnesium, pure zinc, zirconium
Intermediate alloy and yttrium, dysprosium element are placed in melting in electrical crucible, and when melting uses CO2+SF6It is mixed gas protected, smelting temperature
It is 770 DEG C, after standing 15min, is poured (referring to CN105441762A) when pouring at 700 DEG C and be preheated to 180 DEG C.Above-mentioned CO2+SF6
Mixed gas is used for the preparation of magnesium alloy finished product, it is not instructed to can be used for preparing Mg-Zr intermediate alloy.In view of magnesium alloy
Very big with the component difference of Mg-Zr intermediate alloy, those skilled in the art, which do not allow to be readily conceivable that, is used for magnesium zirconium for above-mentioned mixed gas
The production of intermediate alloy.
On the other hand, Mg-Zr intermediate alloy generallys use following method production: by Mg and KCl, ZrCl4In vacuum reduction furnace
Interior fusing vaporizes in vacuum preheating furnace, and is passed through reduction reaction in furnace 8~14 hours, then cool to room temperature to obtain 20~
40% Mg-Zr intermediate alloy.Vacuum equipment is used in the technical process and vaporizes ZrCl4, complex process, and Zr is unevenly distributed
It is even.
Therefore, there is still a need for a kind of production method of Mg-Zr intermediate alloy, to obtain among the magnesium zirconium that Zr is evenly distributed
Alloy.
Summary of the invention
It is an unexpected discovery of the invention that using properly mixed mixed gas, and the adding manner and dosage of zirconium chloride are adjusted,
The Mg-Zr intermediate alloy that the Zr that can be obtained is evenly distributed and is not segregated.The purpose of the present invention is to provide close among a kind of magnesium zirconium
The production method of gold, the Zr in gained alloy are evenly distributed and are not segregated.In order to overcome drawbacks described above, present inventor into
Further investigation is gone.
The present invention provides a kind of production method of Mg-Zr intermediate alloy, includes the following steps: magnesium metal in reacting furnace
Fusing, and be passed through by CO2And SF6The mixed gas of composition, when reacting furnace temperature reaches 750~900 DEG C, low whipping speed is
Under the stirring action of 300~800r/min, zirconium chloride is added in substep, reaction 1~2 hour after the completion of being added；Wherein, mixed gas
In SF6Percent by volume be 0.5vol%~1.5vol%, and the weight ratio of magnesium metal and zirconium chloride be 1:0.1~0.5.
In accordance with the present production process, it is preferable that the substep is added are as follows: every 20~40min, 1/3 weight is added
Zirconium chloride.
In accordance with the present production process, it is preferable that the flow of the mixed gas is 0.2~0.8L/min.
In accordance with the present production process, it is preferable that the pressure of the mixed gas is 0.5~1.5 atmospheric pressure.
In accordance with the present production process, it is preferable that the reacting furnace is not completely enclosed.
In accordance with the present production process, it is preferable that the temperature be 750~800 DEG C, and mixing speed be 500~
600r/min。
In accordance with the present production process, it is preferable that the SF in mixed gas6Percent by volume be 0.8vol%~
1vol%.
In accordance with the present production process, it is preferable that the weight ratio of magnesium metal and zirconium chloride is 1:0.1~0.2.
In accordance with the present production process, it is preferable that further include following steps: the product that reaction obtains is carried out with argon gas
Then blowing refining is cast in mold, and be passed through by CO2And SF6The Mg-Zr intermediate alloy is made in the mixed gas of composition.
In accordance with the present production process, it is preferable that the Fe content of the Mg-Zr intermediate alloy is lower than 0.015wt%, Cu
Content is lower than 0.02wt% lower than 0.008wt% and Si content；The zirconium content of the different parts of the Mg-Zr intermediate alloy it is inclined
Difference is within ± 8%.
The present invention uses properly mixed CO2+SF6Mixed gas is as protective gas, zirconium chloride (ZrCl4) can be fast
Enter in molten magnesium under the action of speed stirring, avoids ZrCl4Vaporization at high temperature, be evenly distributed and be not segregated to obtain Zr
Mg-Zr intermediate alloy.Preferred technical solution according to the present invention, before coming out of the stove using argon gas carry out blowing refining, can well
MgCl2It is separated with alloy, when casting can reduce the burning of alloy using protective gas.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
Zirconium of the invention has the same meaning with Zr, and magnesium has the same meaning with Mg, can be replaced mutually.The present invention
Intermediate alloy be manufacture alloy finished product important source material, but its generally not as alloy finished product use.Among magnesium zirconium of the invention
The main component of alloy is magnesium and zirconium, but does not exclude the presence of a small amount of impurity.
The production method of Mg-Zr intermediate alloy of the invention includes the following steps: to melt magnesium metal in reacting furnace, and
It is passed through by CO2And SF6The mixed gas of composition.The example of reacting furnace includes but is not limited to reduction furnace, be can be used known in the art
Those of.Reacting furnace of the invention does not need to vacuumize, because without vaccum-pumping equipment.Therefore, reacting furnace of the invention is not
It is completely enclosed.
Mixed gas of the invention is only by CO2And SF6Composition does not contain other gases, but a small amount of foreign gas is not precluded
Presence.In the mixed gas, SF6Percent by volume be 0.5vol%~1.5vol%, preferably 0.8vol%~
1vol%, more preferably 0.85vol%~1vol%.It is our surprising discovery that passing through the SF in control mixed gas6Match
Than the distributing homogeneity of the Zr in Mg-Zr intermediate alloy can be improved.
In the present invention, the flow of the mixed gas can be 0.2~0.8L/min, preferably 0.3~0.7L/min,
Preferably 0.5~0.6L/min.The pressure of the mixed gas can be 0.5~1.5 atmospheric pressure, preferably 0.8~1.2
Atmospheric pressure, more preferably 1~1.1 atmospheric pressure.By the flow of mixed gas and the control of/pressure in above range, can control
Reaction process, so as to improve the distributing homogeneity of the Zr in Mg-Zr intermediate alloy.
The production method of Mg-Zr intermediate alloy of the invention further includes following steps: when reacting furnace temperature reaches 750~900
DEG C, preferably 750~800 DEG C when, low whipping speed be 300~800r/min, preferably 500~600r/min stirring action
Under, zirconium chloride is added in substep, reaction 1~2 hour, preferably 1~1.5 hour after the completion of being added.The purpose that substep is repeatedly added
It is to sink to zirconium chloride inside molten magnesium quickly under suitable stirring action, avoids the volatilization loss of zirconium chloride.Maintain reaction
Time is 1~2 hour, can make Mg and ZrCl4Sufficiently reaction.Therefore, the distributing homogeneity quilt of the Zr in Mg-Zr intermediate alloy
It further increases.
In the present invention, the weight ratio of magnesium metal and zirconium chloride is 1:0.1~0.5, preferably 1:0.1~0.2.It is appropriate
The dosage for reducing zirconium chloride, can improve the distributing homogeneity of Zr, but excessive reduction zirconium chloride dosage, then lead to the distribution of Zr
Uniformity is deteriorated.
In the present invention, so-called substep is added are as follows: every 20~40min, 1/3 weight zirconium chloride is added.For example, every
1/3 weight zirconium chloride is added in 30min.Such adding manner, can not only guarantee the distributing homogeneity of Zr, but also life can be improved
Produce efficiency.
Production method of the invention can also include the following steps: the product that reaction obtains carrying out essence of blowing with argon gas
Refining, is then cast in mold, and be passed through by CO2And SF6The Mg-Zr intermediate alloy is made in the mixed gas of composition.Before coming out of the stove
Blowing refining is carried out using argon gas, so that reaction product MgCl2It can be separated well with alloy, to guarantee alloy mass.Out
The alloy melt of furnace is cast in mold, and mold is covered and is passed through by CO2And SF6The mixed gas of composition, until alloy is cooling,
To which Mg-Zr intermediate alloy be made.It is a discovery of the invention that being at this moment passed through mixed gas for improving the Zr of Mg-Zr intermediate alloy
Distributing homogeneity is advantageous.By CO2And SF6Proportion, flow and the pressure of the mixed gas of composition are as previously mentioned, here no longer
It repeats.
In the present invention, the deviation of the zirconium content of the different parts of Mg-Zr intermediate alloy is within ± 8%, preferably ±
Within 5%.So-called deviation indicates the percentage of the zirconium content of different piece and the difference of average zirconium content and average zirconium content.Also
=(zirconium content-of different piece be averaged zirconium content)/average zirconium content that is, deviation.So-called different parts indicate to close among magnesium zirconium
The different sampling points of gold, such as upper, middle and lower.Average zirconium content then indicates the zirconium content of intermediate alloy entirety.Partially
Difference is smaller, indicates that the distributing homogeneity of Zr is better.In addition, the zirconium content of Mg-Zr intermediate alloy can be with 5~19wt%, preferably 5
~15wt%.The Fe content of Mg-Zr intermediate alloy can be lower than 0.008wt% lower than 0.015wt%, Cu content and Si contains
Amount can be lower than 0.02wt%.
Embodiment 1
Magnesium metal is melted in reduction furnace, and is passed through by CO2And SF6Composition mixed gas (flow 0.5L/min,
Pressure is 1 atmospheric pressure, SF6Content is 1vol%).At 750 DEG C, zirconium chloride is added step by step under the stirring of 500r/min
(Mg/ZrCl4=1:0.13), every 30min, the zirconium chloride of 1/3 weight is added, maintains reaction 1 hour after the completion of being added.It comes out of the stove
Preceding to carry out blowing refining with argon gas, alloy melt is cast in mold and is passed through by CO2And SF6(flow is the mixed gas of composition
0.5L/min, pressure are 1 atmospheric pressure, SF6Content is 1vol%), the Mg-Zr intermediate alloy that zirconium content is 5wt% is made.
Embodiment 2
Magnesium metal is melted in reduction furnace, and is passed through by CO2And SF6Composition mixed gas (flow 0.5L/min,
Pressure is 1 atmospheric pressure, SF6Content is 1vol%).At 800 DEG C, zirconium chloride is added step by step under the stirring of 600r/min
(Mg/ZrCl4=1:0.26), every 30min, the zirconium chloride of 1/3 weight is added, maintains reaction 1 hour after the completion of being added.It comes out of the stove
Preceding to carry out blowing refining with argon gas, alloy melt is cast in mold and is passed through by CO2And SF6(flow is the mixed gas of composition
0.5L/min, pressure are 1 atmospheric pressure, SF6Content is 1vol%), the Mg-Zr intermediate alloy that zirconium content is 10wt% is made.
Embodiment 3
Magnesium metal is melted in reduction furnace, and is passed through by CO2And SF6Composition mixed gas (flow 0.5L/min,
Pressure is 1 atmospheric pressure, SF6Content is 1vol%).At 850 DEG C, zirconium chloride is added step by step under the stirring of 600r/min
(Mg/ZrCl4=1:0.4), every 30min, the zirconium chloride of 1/3 weight is added, maintains reaction 1.5 hours after the completion of being added.Out
Stokehold carries out blowing refining with argon gas, and alloy melt is cast in mold and is passed through by CO2And SF6Mixed gas (the flow of composition
It is 1 atmospheric pressure, SF for 0.5L/min, pressure6Content is 1vol%), the Mg-Zr intermediate alloy that zirconium content is 14wt% is made.
Embodiment 4
Magnesium metal is melted in reduction furnace, and is passed through by CO2And SF6Composition mixed gas (flow 0.5L/min,
Pressure is 1 atmospheric pressure, SF6Content is 1vol%).At 900 DEG C, zirconium chloride is added step by step under the stirring of 600r/min
(Mg/ZrCl4=1:0.5), every 30min, the zirconium chloride of 1/3 weight is added, maintains reaction 2 hours after the completion of being added.It comes out of the stove
Preceding to carry out blowing refining with argon gas, alloy melt is cast in mold and is passed through by CO2And SF6(flow is the mixed gas of composition
0.5L/min, pressure are 1 atmospheric pressure, SF6Content is 1vol%), the Mg-Zr intermediate alloy that zirconium content is 19wt% is made.
Comparative example 1
Magnesium metal and sylvite KCl are added in reduction furnace by weight the ratio of 1:1.5, start vacuum system, surely
When reciprocal of duty cycle reaches 1Pa, stop vacuumizing, and be continuously passed through argon gas as protective gas, furnace pressure is+0.006MPa；Down payment
The ratio for belonging to magnesium and zirconium chloride weight ratio 1:2, takes zirconium chloride to be added in preheating furnace, starts vacuum system, works as vacuum degree
Reach 6 × 10-1When Pa, stop vacuumizing, zirconium chloride is heated, through 2 hours, zirconium chloride is heated to 330 DEG C, is made
Zirconium chloride vaporization；While reduction furnace is passed through inert gas, magnesium metal and sylvite KCl are heated, it, will through 5 hours
Material is heated to 950 DEG C, and when material reaches this temperature, the zirconium chloride of vaporization is introduced anti-with molten magnesium in reduction furnace
It answers, continues 8 hours, then, mechanical stirring 1 hour, then will be hung out in its calandria from reduction furnace, it is cooled to room temperature and comes out of the stove,
Obtain Mg-Zr intermediate alloy.
Using inductive coupling high frequency plasma spectrometer (ICP) to the Mg-Zr intermediate alloy of Examples 1 to 4 and comparative example 1
It is measured at normal temperature, intermediate alloy is divided into upper, middle and lower, separately sampled measurement zirconium content, test result ginseng
It is shown in Table 1 and 2.
ICP: French large profits Bagong department (HORIBA JY), ULTIMA 2ICP inductive coupling plasma emission spectrograph,
Sample is with dissolving with hydrochloric acid, in diluted hydrochloric acid medium, directly with argon plasma light source activation, carries out spectroscopic assay.
Zirconium distributing homogeneity in table 1, intermediate alloy
| Number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 |
| Average zirconium content/% | 5 | 10 | 14 | 19 | 30 |
| Zirconium content/the % on top | 4.91 | 9.78 | 14.10 | 18.67 | 25.62 |
| Zirconium content/the % at middle part | 5.16 | 9.92 | 14.32 | 19.23 | 28.75 |
| Zirconium content/% of lower part | 5.32 | 10.25 | 14.58 | 19.64 | 33.21 |
Impurity content in table 2, intermediate alloy
| Number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 |
| Fe content/% | 0.0026 | 0.0041 | 0.0018 | 0.0134 | 0.0486 |
| Cu content/% | 0.0031 | 0.0068 | 0.0053 | 0.0044 | 0.0527 |
| Si content/% | 0.0121 | 0.0095 | 0.0134 | 0.0187 | 0.0635 |
Present invention is not limited to the embodiments described above, without departing from the essence of the present invention, this field skill
Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.
Claims (10)
1. a kind of production method of Mg-Zr intermediate alloy, which comprises the steps of: melt magnesium metal in reacting furnace
Change, and is passed through by CO2And SF6The mixed gas of composition, when reacting furnace temperature reaches 750~900 DEG C, low whipping speed 300
Under the stirring action of~800r/min, zirconium chloride is added in substep, reaction 1~2 hour after the completion of being added；Wherein, in mixed gas
SF6Percent by volume be 0.5vol%~1.5vol%, and the weight ratio of magnesium metal and zirconium chloride be 1:0.1~0.5；
Wherein, reacting furnace is not completely enclosed.
2. production method according to claim 1, which is characterized in that the substep is added are as follows: every 20~40min, adds
Enter 1/3 weight zirconium chloride.
3. production method according to claim 1, which is characterized in that the flow of the mixed gas is 0.2~0.8L/
min。
4. production method according to claim 1, which is characterized in that the pressure of the mixed gas is 0.5~1.5 big
Air pressure.
5. production method according to claim 4, which is characterized in that the pressure of the mixed gas is 0.8~1.2 big
Air pressure.
6. described in any item production methods according to claim 1~5, which is characterized in that the temperature is 750~800 DEG C, and
Mixing speed is 500~600r/min.
7. production method according to claim 6, which is characterized in that the SF in mixed gas6Percent by volume be
0.8vol%~1vol%.
8. production method according to claim 7, which is characterized in that the weight ratio of magnesium metal and zirconium chloride be 1:0.1~
0.2。
9. described in any item production methods according to claim 1~5, which is characterized in that further include following steps: will react
The product arrived carries out blowing refining with argon gas, is then cast in mold, and is passed through by CO2And SF6The mixed gas of composition, system
Obtain the Mg-Zr intermediate alloy.
10. production method according to claim 9, which is characterized in that the zirconium of the different parts of the Mg-Zr intermediate alloy
The deviation of content is within ± 8%.
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Address after: No.36, Huanghe street, rare earth high tech Zone, Baotou City, Inner Mongolia Autonomous Region Patentee after: Baotou Rare Earth R&D Center, Chinese Academy of Sciences Patentee after: Lizhong Sitong light alloy Group Co.,Ltd. Patentee after: Changchun Institute of Applied Chemistry Chinese Academy of Sciences Address before: 014030 No. 36, Huanghe street, rare earth R & D zone, Qingshan District, Baotou City, Inner Mongolia Autonomous Region Patentee before: Baotou Rare Earth R&D Center, Chinese Academy of Sciences Patentee before: HEBEI SITONG NEW METAL MATERIAL Co.,Ltd. Patentee before: Changchun Institute of Applied Chemistry Chinese Academy of Sciences |