CN106756180B - A kind of calcium/magnesia grain refiner and its preparation method and application - Google Patents
A kind of calcium/magnesia grain refiner and its preparation method and application Download PDFInfo
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- CN106756180B CN106756180B CN201611111273.9A CN201611111273A CN106756180B CN 106756180 B CN106756180 B CN 106756180B CN 201611111273 A CN201611111273 A CN 201611111273A CN 106756180 B CN106756180 B CN 106756180B
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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
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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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Abstract
The invention discloses a kind of calcium/magnesia grain refiners and preparation method and application, belong to non-ferrous metal technical field.Grain refiner of the present invention has apparent core-shell structure, and wherein calcium constituent is distributed in the periphery of magnesium oxide particle；Particle size distribution is concentrated mainly on 200nm or so.Specifically preparation method is：Under sulfur hexafluoride and nitrogen mixed gas protection, pure magnesium is heated to half solidification state；Lime powder is added in, stirring makes it be uniformly blended into half solidifying solid magnesium liquid；Raising furnace temperature to magnesium liquid is completely melt, target product is obtained after cast iron casting molding is poured into after quiescence in high temperature.The grain refiner of the present invention is with obvious effects to magnesium and magnesium alloy grains；And remain to the grain refining effect kept in the case where different solidification cooling conditions or high temperature stand do not stir for a long time；The grain refiner manufacturing cost is relatively low, and adding technology is simple, suitable for industrialized production.
Description
Technical field
The invention belongs to non-ferrous metal technical fields, and in particular to a kind of calcium/magnesia grain refiner and its preparation side
The application of method and the fining agent in magnesium and magnesium alloy.
Background technology
The equiax crystal of fine uniform is magnesium and the best as-cast structure of magnesium alloy materials, to obtain this tissue, it is necessary to logical
Cross the miniaturization processing of different means crystal grain thinnings, i.e. crystalline structure.Its means includes adding in various intermediate alloys during liquid
Fining agent or by extraneous energy, such as mechanical oscillation, electromagnetic agitation, high speed shear, ultrasonication refine α-Mg matrixes,
So as to significantly improve the mechanical property of magnesium material and process industrial art performance.Crystal grain refinement can improve intensity and the modeling of material simultaneously
Property, it is the important channel for obtaining high-quality magnesium ingot, improving magnesium material amount.Current 90% magnesium alloy mainly uses under as cast condition, because
The crystal grain refinement of this magnesium alloy cast tissue is particularly important.Special equipment and technique are needed by extraneous energy, in practical work
It is relatively difficult to achieve in industry production, and also limited by working condition etc., effect is limited, and process is difficult to control.In industrial production
Under the conditions of, it is most simple and effective method and the important component of Serum Magnesium treatment technology only to add fining agent.Mesh
The crystal grain refinement means of preceding industrial magnesium and its alloy divide two kinds of situations by alloy species：The first situation is containing almag
Crystal grain refinement.Generally using overheat, carbon or carbon compound addition.The stability of such fining agent grain refining effect limits it
Large-scale application industrially.The second situation is free from the crystal grain refinement of almag.Common use is added among magnesium zirconium
Alloy approach realizes crystal grain refinement.But in practical applications, the fining agent is there is also noble metal zirconium dosage is big, and zr element is chemically
Matter is active, the problems such as easily failure with other element reactions.
Invention content
The present invention is for existing magnesium and its alloy grain refinement deficiency and defect, it is proposed that a kind of calcium/magnesia crystal grain is thin
Agent, to there is stronger grain refining effect to magnesium and its alloy, performance is stable simultaneously, is easy to industrialize.
In order to solve the above technical problems, what the present invention was achieved by the following technical programs.
The present invention provides a kind of grain refiner, forming core particle is typical core-shell structure, i.e. calcium constituent is distributed in
The periphery of magnesium oxide particle, particle diameter distribution is uniform, average grain diameter 200nm.
Invention also provides the preparation methods of above-mentioned grain refiner, are as follows：Crucible toward after cleaning
It is interior to add in pure magnesium, under sulfur hexafluoride and nitrogen mixed gas protection, it is heated to half solidification state；It is a small amount of repeatedly to add in calcium oxide powder
End, average particle size range are 0.1~1 μm；Lime powder addition CaO by weight ratio:Mg=1~5:100；Add every time
Enter that calcium oxide powder is last, be sufficiently stirred to coagulate in solid magnesium liquid to ensure that the lime powder added in is uniformly blended into half；After of continuing rising
High furnace temperature stands heat preservation and is completely melt to magnesium liquid to 680~720 DEG C, is stirred well to added lime powder more uniform distribution
In Serum Magnesium；Then melt is poured into cylindrical cast iron casting mould, casting cycle leads to protective gas, ensures melt in the casting stage
It is missing of ignition, target product is obtained after air natural cooling：Calcium/magnesia grain refiner.
Above-mentioned grain refiner can be used for the crystal grain refinement of magnesium or magnesium alloy.In this application, the grain refiner accounts for
The mass percent of magnesium or magnesium alloy is 0.1~1%.
The principles of science of the present invention：
Additional lime powder is unstable in pure magnesium melt, easily generates magnesia and calcium, wherein calcium by pure magnesium-reduced
Element adsorbs the mgo surface in reduction in situ, forms typical core-shell structure.The calcium constituent adsorbed in mgo surface leads to
It crosses to form nucleation ability of the transition intermediate compound form raising magnesia to magnesium and its alloy, plays and effectively refine magnesium crystal grain
Effect.
Compared with prior art, the present invention has following technique effect：
1st, the preparation method of fining agent of the present invention is simple and easy to control, cheap, it is easy to accomplish industrialized production.
2nd, the grain refiner particle diameter distribution that prepared by the present invention is uniform, and addition manner is simple.
3rd, the grain refiner that prepared by the present invention is apparent to the grain refining effect of magnesium and its alloy.
4th, grain refiner prepared by the present invention stands what is do not stirred for a long time in different solidification cooling conditions or high temperature
In the case of remain to the grain refining effect kept.
Description of the drawings
Fig. 1 is calcium/magnesia grain refiner particulate scan transmission electron microscope picture prepared by the embodiment of the present invention 1；
Wherein：(a) it is calcium/magnesia grain refiner particle micro-organization chart；(b) it is calcium constituent distribution map, it can by figure
Know, calcium constituent is distributed in the periphery of magnesium oxide particle.
Fig. 2 is that (crystal grain is thin for macrostructure's comparison diagram of pure Serum Magnesium sample after TP1 casts before and after adding in grain refiner
Agent is prepared by the embodiment of the present invention 1, similarly hereinafter)；
Wherein：(a) it is the macrostructure of pure Serum Magnesium sample after TP1 casts；(b) be add in mass fraction be 0.1%
Grain refiner pure Serum Magnesium sample after TP1 casts macrostructure.
Fig. 3 is the microstructure comparison diagram of Mg-3Al alloy melts sample after TP1 casts before and after addition grain refiner；
Wherein：(a) it is the microstructure of Mg-3Al alloy melts sample after TP1 casts；(b) it is to add in mass fraction to be
The microstructure of Mg-3Al alloy melts sample after TP1 casts of 0.1% grain refiner.
Fig. 4 is macrostructure's comparison diagram of pure Serum Magnesium sample after wedge-shaped die is cast before and after addition grain refiner；
Wherein：(a) it is the macrostructure of pure Serum Magnesium sample after wedge-shaped die is cast；(b) it is to add in mass fraction to be
The macrostructure of pure Serum Magnesium sample after wedge-shaped die is cast of 0.1% grain refiner.
Fig. 5 is that the pure Serum Magnesium quiescence in high temperature different time of the grain refiner sampling that addition mass fraction is 0.1% (divides
0.5h (a), 1.5h (b), 2.5h (c), 6.5h (d) are not corresponded to) macrostructure's comparison diagram of sample after TP1 casts.
Specific embodiment
The present invention is described in detail, but the present invention is not limited to following embodiments below in conjunction with specific embodiments and the drawings.
First, the preparation of grain refiner
Embodiment 1
Pure magnesium is added in the crucible after cleaning, under sulfur hexafluoride and nitrogen mixed gas protection, is heated to half solidification
State；A small amount of repeatedly to add in lime powder, average grain diameter is 0.1 μm；Lime powder addition CaO by weight ratio:Mg
=1:100；It is last that calcium oxide powder is added in every time, is sufficiently stirred to ensure that it is solidifying solid that the lime powder added in is uniformly blended into half
In magnesium liquid；Continue to increase furnace temperature to 680 DEG C, stand heat preservation and be completely melt to magnesium liquid, be stirred well to added lime powder compared with
It is evenly distributed in Serum Magnesium；30min is kept the temperature at 680 DEG C, melt pours into cylindrical cast iron casting mould (a diameter of 10mm)；It cast
Journey leads to protective gas, ensures that melt is missing of ignition in the casting stage, air natural cooling obtains grain refiner of the invention.
Embodiment 2
Pure magnesium is added in the crucible after cleaning, under sulfur hexafluoride and nitrogen mixed gas protection, is heated to half solidification
State；A small amount of repeatedly to add in lime powder, average grain diameter is 1 μm；Lime powder addition CaO by weight ratio:Mg=
1:100；It is last that calcium oxide powder is added in every time, is sufficiently stirred and is coagulated solid magnesium to ensure that the lime powder added in is uniformly blended into half
In liquid；Continue to increase furnace temperature to 680 DEG C, stand heat preservation and be completely melt to magnesium liquid, it is more equal to be stirred well to added lime powder
It is even to be distributed in Serum Magnesium；30min is kept the temperature at 680 DEG C, melt pours into cylindrical cast iron casting mould (a diameter of 10mm)；Casting cycle
Logical protective gas ensures that melt is missing of ignition in the casting stage, and air natural cooling obtains grain refiner of the invention.
Embodiment 3
Pure magnesium is added in the crucible after cleaning, under sulfur hexafluoride and nitrogen mixed gas protection, is heated to half solidification
State；A small amount of repeatedly to add in lime powder, average particle size range is 0.1 μm；Lime powder addition is by weight ratio
CaO:Mg=5:100；It is last that calcium oxide powder is added in every time, is sufficiently stirred to ensure that it is solidifying that the lime powder added in is uniformly blended into half
In solid magnesium liquid；Continue to increase furnace temperature to 680 DEG C, stand heat preservation and be completely melt to magnesium liquid, be stirred well to added calcium oxide
Powder more uniform distribution is in Serum Magnesium；30min is kept the temperature at 680 DEG C, melt pours into cylindrical cast iron casting mould (a diameter of 10mm)；
Casting cycle leads to protective gas, ensures that melt is missing of ignition in the casting stage, air natural cooling obtains grain refiner of the invention.
Embodiment 4
Pure magnesium is added in the crucible after cleaning, under sulfur hexafluoride and nitrogen mixed gas protection, is heated to half solidification
State；A small amount of repeatedly to add in lime powder, average particle size range is 0.1 μm；Lime powder addition is by weight ratio
CaO:Mg=5:100；It is last that calcium oxide powder is added in every time, is sufficiently stirred to ensure that it is solidifying that the lime powder added in is uniformly blended into half
In solid magnesium liquid；Continue to increase furnace temperature to 720 DEG C, stand heat preservation and be completely melt to magnesium liquid, be stirred well to added calcium oxide
Powder more uniform distribution is in Serum Magnesium；30min is kept the temperature at 680 DEG C, melt pours into cylindrical cast iron casting mould (a diameter of 10mm)；
Casting cycle leads to protective gas, ensures that melt is missing of ignition in the casting stage, air natural cooling obtains grain refiner of the invention.
Embodiment 5
Pure magnesium is added in the crucible after cleaning, under sulfur hexafluoride and nitrogen mixed gas protection, is heated to half solidification
State；A small amount of repeatedly to add in lime powder, average particle size range is 0.1 μm；Lime powder addition is by weight ratio
CaO:Mg=5:100；It is last that calcium oxide powder is added in every time, is sufficiently stirred to ensure that it is solidifying that the lime powder added in is uniformly blended into half
In solid magnesium liquid；Continue to increase furnace temperature to 680 DEG C, stand heat preservation and be completely melt to magnesium liquid, be stirred well to added calcium oxide
Powder more uniform distribution is in Serum Magnesium；30min is kept the temperature at 720 DEG C, melt pours into cylindrical cast iron casting mould (a diameter of 10mm)；
Casting cycle leads to protective gas, ensures that melt is missing of ignition in the casting stage, air natural cooling obtains grain refiner of the invention.
2nd, the comparative test of grain refiner performance
Embodiment I：The pure magnesium of business level is added in into low-carbon steel crucible, the melting in electrical crucible, be passed through sulfur hexafluoride and
Nitrogen mixed gas is protected, and smelting temperature is 680 DEG C；After the fusing of pure magnesium, 680 DEG C stand isothermal holding 30min；Deslagging degasification
Afterwards, TP-1 ingot castings are cast into 680 DEG C；After cooling and demolding, the pure magnesium ingot casting of gained is splitted along longitudinal section, is corroded and is observed macroscopical group
It knits.
Comparative example I：This example production stage is substantially the same manner as Example 1, be a difference in that treat pure magnesium melt completely, stand and
After deslagging degasification, the grain refiner disclosed by the invention prepared by 1 method of embodiment is added in, in an amount of from pure magnesium mass fraction
0.1%, it is sufficiently stirred, 680 DEG C are cast into TP-1 ingot castings；After cooling and demolding, gained magnesium alloy ingot is splitted along longitudinal section, corrosion
And observe metallurgical microstructrue.
Embodiment II：Mg-3Al magnesium alloys are added in into low-carbon steel crucible, the melting in electrical crucible is passed through sulfur hexafluoride
It is protected with nitrogen mixed gas, smelting temperature is 680 DEG C；After magnesium alloy fusing, 680 DEG C stand isothermal holding 30min；Deslagging
After degasification, 680 DEG C are cast into TP-1 ingot castings；After cooling and demolding, gained magnesium alloy ingot is splitted along cross section, is corroded and is observed macro
See tissue.
Comparative example II：This example production stage is substantially the same manner as Example 2, is a difference in that and treats that Mg-3Al magnesium alloys are completely molten
After solution, standing and deslagging degasification, the grain refiner disclosed by the invention prepared by 1 method of embodiment is added in, is closed in an amount of from magnesium
The 0.1% of golden mass fraction, is sufficiently stirred, and 680 DEG C are cast into TP-1 ingot castings；After cooling and demolding, gained magnesium alloy ingot edge is horizontal
Section corrodes and observes metallurgical microstructrue.
Embodiment III：The pure magnesium of business level is added in into low-carbon steel crucible, the melting in electrical crucible, be passed through sulfur hexafluoride and
Nitrogen mixed gas is protected, and smelting temperature is 680 DEG C；After the fusing of pure magnesium, 680 DEG C stand isothermal holding 30min；Deslagging degasification
Afterwards, casting wedge shape mould is poured into for 680 DEG C；After cooling and demolding, the pure magnesium ingot casting of gained is splitted along longitudinal section, is corroded and is observed macroscopical group
It knits.
Comparative example III：This example production stage is substantially the same manner as Example 3, is a difference in that and treats that pure magnesium is melted, stood completely
And after deslagging degasification, the grain refiner disclosed by the invention prepared by 1 method of embodiment is added in, in an amount of from pure magnesium mass fraction
0.1%, be sufficiently stirred, 680 DEG C pour into casting wedge shape mould；After cooling and demolding, the pure magnesium ingot casting of gained is splitted along longitudinal section, corrosion
And observe metallurgical microstructrue.
Embodiment IV：The pure magnesium of business level is added in into low-carbon steel crucible, the melting in electrical crucible passes through SF6/N2Mixing
Gas shield, smelting temperature are 680 DEG C；Melted completely after pure magnesium, stand and deslagging degasification after, add in disclosed by the invention by real
The grain refiner of 1 method of example preparation is applied, in an amount of from the 0.1% of pure magnesium mass fraction, rear quiescence in high temperature is sufficiently stirred, selects respectively
0.5h, 1.5h, 2.5h and 6.5h is taken not to be cast into TP-1 ingot castings under stirring state；After cooling and demolding.Gained magnesium ingot casting is cut along vertical
Face is splitted, and is corroded and is observed metallurgical microstructrue.
The results show that calcium using the present invention/magnesia grain refiner has apparent core-shell structure, wherein calcium constituent
It is distributed in the periphery of magnesium oxide particle；Grain diameter is concentrated mainly on 200nm or so (referring to Fig. 1)；The grain refiner is pure
Thinning effect is preferable in magnesium, and grain structure is changed into equiax crystal by typical column crystal (referring to Fig. 2)；The grain refiner exists
Thinning effect is preferable in Mg-3Al magnesium alloys, and average grain size is reduced to 100 μm (referring to Fig. 3) by 400 μm；The crystal grain refinement
The crystal grain that agent remains to keep in the case where solidification cooling different condition (referring to Fig. 4) or high temperature stand do not stir for a long time is thin
Change effect (referring to Fig. 5).
Claims (2)
1. a kind of calcium/magnesia grain refiner, it is characterised in that：The fining agent has core-shell structure, and calcium constituent is distributed in oxygen
Change the periphery of magnesium granules, particle diameter distribution is uniform, average grain diameter 200nm；
The preparation of the calcium/magnesia grain refiner includes the following steps：
(1) pure magnesium is added in the crucible after cleaning, under sulfur hexafluoride and nitrogen mixed gas protection, is heated to half solidification
State；
(2) a small amount of that lime powder is repeatedly added in crucible, average particle size range is 0.1~1 μm；Lime powder adds in
Measure CaO by weight ratio:Mg=1~5:100；It is last that calcium oxide powder is added in every time, is sufficiently stirred to ensure the calcium oxide added in
Powder is uniformly blended into half and coagulates in solid magnesium liquid；
(3) continue to increase furnace temperature to 680~720 DEG C, stand heat preservation and be completely melt to magnesium liquid, be stirred well to added calcium oxide powder
End is evenly distributed in Serum Magnesium；Then melt is poured into cylindrical cast iron casting mould, casting cycle leads to protective gas, ensures melt
Missing of ignition in the casting stage, natural cooling obtains calcium/magnesia grain refiner under air.
2. calcium as described in claim 1/application of the magnesia grain refiner in magnesium or magnesium alloy, it is characterised in that：Institute
It is 0.1~1% to state grain refiner and account for magnesium or the mass percent of magnesium alloy.
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| CN201611111273.9A CN106756180B (en) | 2016-12-01 | 2016-12-01 | A kind of calcium/magnesia grain refiner and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107988500A (en) * | 2017-12-11 | 2018-05-04 | 安徽工业大学 | Application of the barium monoxide as grain refiner in magnesium or magnesium alloy |
| CN109022861B (en) * | 2018-09-30 | 2020-09-22 | 华南理工大学 | Grain refinement method of Mg-Al series alloy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135014A (en) * | 2007-10-11 | 2008-03-05 | 武汉理工大学 | Mg-Al series alloy composite grain refiner and method for making same |
| CN101812607A (en) * | 2010-04-22 | 2010-08-25 | 东北轻合金有限责任公司 | Magnesium alloy refiner and preparation method thereof |
| CN102206765A (en) * | 2010-03-29 | 2011-10-05 | 韩国生产技术研究院 | Magnesium alloy for room temperature and manufacturing method thereof |
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- 2016-12-01 CN CN201611111273.9A patent/CN106756180B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135014A (en) * | 2007-10-11 | 2008-03-05 | 武汉理工大学 | Mg-Al series alloy composite grain refiner and method for making same |
| CN102206765A (en) * | 2010-03-29 | 2011-10-05 | 韩国生产技术研究院 | Magnesium alloy for room temperature and manufacturing method thereof |
| CN101812607A (en) * | 2010-04-22 | 2010-08-25 | 东北轻合金有限责任公司 | Magnesium alloy refiner and preparation method thereof |
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