CN101629261B - Rare earth flame resistance magnesium alloy and preparation method thereof - Google Patents
Rare earth flame resistance magnesium alloy and preparation method thereof Download PDFInfo
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- CN101629261B CN101629261B CN2009100701138A CN200910070113A CN101629261B CN 101629261 B CN101629261 B CN 101629261B CN 2009100701138 A CN2009100701138 A CN 2009100701138A CN 200910070113 A CN200910070113 A CN 200910070113A CN 101629261 B CN101629261 B CN 101629261B
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Abstract
The invention provides a rare earth flame resistance magnesium alloy and a preparation method thereof and relates to a magnesium-based alloy adopting rare earth metal as main component; and the atom percentage of the elements of the alloy is Mg96.0-98.19Y0.31-0.5Dy1.5-3.5. The preparation method comprises the following steps: first weighting three raw materials, namely pure magnesium, Mg-Y preliminary alloy containing 29.05% of Y and Mg-Dy preliminary alloy containing 29.025% of Dy according to the weight percent of the elements of the alloy, heating and smelting at 600-720 DEG C, intermittently injecting mixed protective gases containing 99.5vol.% of CO2 and 0.5vol.% of SF6 at about 600 DEG C, 650 DEG C and 720 DEG C, and finally casting to obtain Mg96.0-98.19Y0.31-0.5Dy1.5-3.5 flame resistance magnesium alloy product. The product has very high purity and higher flame resistance property.
Description
Technical field
Technical scheme of the present invention relates to the Magnuminium that rare earth metal is made time main component, specifically a kind of rare earth flame resistance magnesium alloy and preparation method thereof.
Background technology
The position of Mg in periodictable is in the scope of basic metal, and its extranuclear electron belongs to less, and this has determined Mg to have very strong chemically reactive.Mg is easy to react with the medium with oxidisability, thereby makes product and member based on Mg be greatly limited in application.Yet, Mg has the not available good characteristic of some other metals: light weight, high specific strength and high specific stiffness, good diamagnetism and damping property, excellent chip processibility and easy characteristics such as recovery, so magnesium alloy has irreplaceable advantage in fields such as aviation, traffic and electronics.
Be directed to the shortcoming of magnesium and the easy oxidizing fire of magnesium alloy, so far, researcher was successively studied the preparation method of multiple antiflaming magnesium alloy both at home and abroad.These methods roughly are divided into: flux-covering, gas protection method and alloying ignition-proof method.These three kinds of methods have been brought some inevitable side effects when playing the effect of raising magnesium alloy flame-proof.Flux in the flux-covering adopts the mixture of villaumite or villaumite more, in the process of melting magnesium alloy, because the density of villaumite is big, the villaumite that adds can constantly sink to the bottom, the adding that need not stop, this has caused being involved in of more inclusiones undoubtedly, in addition, villaumite is deleterious, threatens for health of human body and safety; Though gas protection method has solved operational complicacy, but gases used is rare gas or some mixed gass that contain S, the rare gas cost is high and rare, be unsuitable for extensively promoting the use of, and the gas that contains S can produce some poisonous gases or have the gas of superpower Greenhouse effect, produces to produce with safety type, environment-friendly type that the whole world proposes and conflicts; The alloying ignition-proof method is the present comparatively preparation method of ideal antiflaming magnesium alloy, yet in all ignition-proof elements, list just improves flame retardant resistance, the best results of Be and Ca, but Be is a toxic substance, and the adding of calcium makes the mechanical property of magnesium alloy reduce greatly.In addition, except the preparation method of above-mentioned three kinds of common antiflaming magnesium alloys, also having a kind of is the renewal of producing apparatus.The external main equipment of having developed the vacuum melting magnesium alloy, but its fund input in early stage is huge, and because the restriction of China's metallurgical equipment technology and enterprise model, this method can't be used at home.
China is rare earth resources big country, and the investigators of China more and more pay attention to and constantly the research and development rare earth is for the special role of metallic substance for this reason, and rare earth can not only purify molten metal, the slagging-off exhaust, and can also optimize the performance of material.In order to make this material with good characteristic of Mg obtain bigger utility value, the investigators of China have also carried out positive research and development for the effect of rare earth in magnesium alloy.
CN101376938 discloses a kind of novel flame-retardant high-strength heat-resistant magnesium alloy and preparation method thereof, is Al-Ca master alloy, Al-RE master alloy and Al-Sr master alloy are joined among the fused magnesium alloy AZ91D; CN1400328 has disclosed strong-toughness fire-resisting magnesium alloy, and its component comprises Al, Zn, Mn, RE and Mg; The fireproof cast magnesium alloy of CN1540016 report, its component is Al, Zn, Mn, RE, Be and Mg.RE in the above-mentioned patent documentation is a mixed rare-earth elements.The composition of as seen existing disclosed rare earth class antiflaming magnesium alloy all is to be that alloy is master alloy and other master alloy that matrix adds multiple mixed rare-earth elements then with magnesium alloy Mg-Al system commonly used and Mg-Zn, also cause the preparation method of existing disclosed rare earth class antiflaming magnesium alloy in the melting preparation process, can be involved in some impurity inevitably thus, and the thermotolerance of its antiflaming magnesium alloy that makes is that burning-point is still waiting further raising.
CN200910069793.1 flame-retardant foam magnesium alloy and preparation method thereof is disclosed to be that to adopt the flux foaming two-step process to make magnesium yttrium dysprosium ternary alloy be the flame-retardant foam magnesium alloy product of body material, and its preparation technology and the product structure performance that makes have essential difference with the antiflaming magnesium alloy of non-foam shape.
Summary of the invention
Technical problem to be solved by this invention is: a kind of rare earth flame resistance magnesium alloy and preparation method thereof is provided, it is to be matrix with pure magnesium, it is added simultaneously with Mg-Y and Mg-Dy master alloy, make the prepared magnesium yttrium of its mode that melts together dysprosium ternary antiflaming magnesium alloy, the atomic percent of its composition is: Mg
96.0～98.19Y
0.31～0.5Dy
1.5～3.5This method has overcome the preparation method who has disclosed rare earth class antiflaming magnesium alloy now can be involved in some impurity inevitably in the melting preparation process shortcoming, and the thermotolerance of its antiflaming magnesium alloy that makes is that burning-point is further enhanced.
The present invention solves this technical problem the technical scheme that is adopted: a kind of rare earth flame resistance magnesium alloy is a magnesium yttrium dysprosium ternary antiflaming magnesium alloy, and the atomic percent of its component is Mg
96.0～98.19Y
0.31～0.5Dy
1.5～3.5
The preparation method of above-mentioned a kind of rare earth flame resistance magnesium alloy the steps include:
The first step, batching
Mass percent by component is that Mg: Y: Dy=96.0～98.19: 0.31～0.5: 1.5～3.5 take by weighing pure magnesium, Mg-Y master alloy and Mg-Dy master alloy raw material, wherein, the mass percent that the Mg-Y master alloy contains Y be 29.05% all the other are Mg, the mass percent that the Mg-Dy master alloy contains Dy be 29.025% all the other are Mg;
Second step, the melting of rare earth flame resistance magnesium alloy
Crucible is preheated to 500 ℃ of taking-ups in the crucible type resistance furnace; the pure magnesium that the first step is taken by weighing; in Mg-Y master alloy and the full raw material of Mg-Dy master alloy portion this crucible of disposable adding; again this crucible is put into the crucible type resistance furnace rapidly; and feed shielding gas at once one time; in 600～720 ℃ of heating down of temperature; at 600 ℃; 650 ℃ and 720 ℃ are carried out intermittence and feed shielding gas; cause whole raw material fusings; more than the fusing point of magnesium, carry out mechanical stirring and make the rare earth element homodisperse; the residue that will float over when stirring above this liquid magnesium alloy removes; carry out the melting of rare earth flame resistance magnesium alloy, described shielding gas is 99.5vol.%CO
2+ 0.5vol.%SF
6Mixed gas;
In the 3rd step, be cast into the antiflaming magnesium alloy goods
With the rare earth flame resistance magnesium alloy liquid of the temperature in the crucible in the second step crucible type resistance furnace 720 ℃ melting, be heated to 740 ℃, left standstill 10 minutes, be cast to then in the metallic mould, the atomic percent that promptly makes component is Mg
96.0～98.19Y
0.31～0.5Dy
1.5～3.5The antiflaming magnesium alloy goods.
Above-mentioned a kind of rare earth flame resistance magnesium alloy and preparation method thereof, described pure magnesium raw material are that purity is that mass percent is 99.95% pure magnesium.
Above-mentioned a kind of rare earth flame resistance magnesium alloy and preparation method thereof, described Mg-Y master alloy and Mg-Dy master alloy raw material are bought in Inner Mongol rare earth research institute, and then by general commercial acquisition, used equipment is general to described pure magnesium raw material.
The invention has the beneficial effects as follows: compared with prior art, marked improvement of the present invention is;
(1) antiflaming magnesium alloy that makes of the inventive method has very high purity, thereby various excellent property.
1. the mother metal selected for use of prior art CN101376938 is AZ91D, it is the magnesium alloy of refining through a procedure by pure magnesium commonly used, inevitably can be involved in some impurity in the melting preparation process, the mother metal that the present invention selects for use is pure magnesium, has avoided being involved in of impurity.
2. the used master alloy of prior art CN101376938 has three kinds of Al-Ca master alloy, Al-RE master alloy and Al-Sr master alloys, and the used master alloy of the present invention has only two kinds of Mg-Y master alloy and Mg-Dy master alloys.The master alloy kind of selecting for use is many more, can cause the purity of liquid magnesium alloy low more during melting.
3. in the preparation process of magnesium alloy, what prior art CN101376938 adopted is at 740 ℃, adds the master alloy of preheating after the mother metal AZ91D fusing again.Under 740 ℃ high temperature, the gas that the surface of liquid magnesium alloy is easy in the absorbed air reacts, the impurity of liquid magnesium alloy is increased, when middle alloy adds fashionable, can stir the liquid magnesium alloy surface, make the gas of absorption be rolled into liquid magnesium alloy inside, thereby reduce the performance of the antiflaming magnesium alloy of preparing.The mode that the inventive method adopts mother metal and master alloy to add together is involved in gas when having avoided secondary to add master alloy, thereby guarantees that liquid magnesium alloy is pure, guarantees the premium properties of the antiflaming magnesium alloy prepared thus.
(2) burning-point of the antiflaming magnesium alloy that makes of the inventive method improves, and promptly flame retardant properties improves.
The antiflaming magnesium alloy that the inventive method is made carries out flame retardant test, and the result is that its burning-point has improved about 200 ℃ than pure magnesium burning-point, and the mean value of burning-point has reached more than 850 ℃.This result is better than the fire-retardant general effect of the antiflaming magnesium alloy of CN101376938, CN1400328 and CN1540016 report.In test burning-point process; when the antiflaming magnesium alloy part that the inventive method makes has Mars to glimmer; itself self-regeneration rapidly; stoped incendiary further to carry out; further heating; after the antiflaming magnesium alloy fusing that the inventive method makes, its surperficial oxide film toughness is fine, has protected the liquid magnesium alloy of molten state effectively.
Feed a part protection gas when (3) the inventive method is implemented in some characteristic temperatures and stop the supple of gas or steam then, promptly, carry out intermittence at 600 ℃, 650 ℃ and 720 ℃ and feed shielding gas, prevent the deep oxidation of raw material in 600～720 ℃ of heating down of temperature.Because that the inventive method adopts is CO
2+ SF
6The mode that hybrid protection gas, this intermittent type feed shielding gas has significantly reduced because SF
6And the Greenhouse effect that cause have also reduced production cost simultaneously effectively, and will endanger reduction aspect environmental protection and the personnel safety.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the high power metallograph of the antiflaming magnesium alloy goods that make of the embodiment of the invention 1.
Fig. 2 is the low power metallograph of the antiflaming magnesium alloy goods that make of the embodiment of the invention 1.
Embodiment
Embodiment 1
The first step, batching
Mass percent by component is Mg: Y: Dy=97.65: take by weighing pure magnesium, Mg-Y master alloy and Mg-Dy master alloy raw material at 0.35: 2.0, wherein, the mass percent that the Mg-Y master alloy contains Y be 29.05% all the other are Mg, the mass percent that the Mg-Dy master alloy contains Dy be 29.025% all the other are Mg, used pure magnesium is commercial commodity, and Mg-Y master alloy and Mg-Dy master alloy are available from Inner Mongol rare earth research institute;
Second step, the melting of rare earth flame resistance magnesium alloy
Crucible is preheated to 500 ℃ of taking-ups in the crucible type resistance furnace; the pure magnesium that the first step is taken by weighing; in Mg-Y master alloy and the full raw material of Mg-Dy master alloy portion this crucible of disposable adding; again this crucible is put into the crucible type resistance furnace rapidly; and feed shielding gas at once one time; in 600～720 ℃ of heating down of temperature; at 600 ℃; 650 ℃ and 720 ℃ are carried out intermittence and feed shielding gas; cause whole raw material fusings; more than the fusing point of magnesium, carry out mechanical stirring and make the rare earth element homodisperse; the residue that will float over when stirring above this liquid magnesium alloy removes; carry out the melting of rare earth flame resistance magnesium alloy, described shielding gas is 99.5vol.%CO
2The mixed gas of+0.5vol.%SF6;
In the 3rd step, be cast into the antiflaming magnesium alloy goods
With the rare earth flame resistance magnesium alloy liquid of the temperature in the crucible in the second step crucible type resistance furnace 720 ℃ melting, be heated to 740 ℃, left standstill 10 minutes, be cast to then in the metallic mould, the atomic percent that promptly makes component is Mg
97.65Y
0.35Dy
2.0The antiflaming magnesium alloy goods.
Fig. 1 is 500 times of metallographs of the antiflaming magnesium alloy goods that make of the embodiment of the invention 1, and Fig. 2 is 200 times of metallographs of the antiflaming magnesium alloy goods that make of the embodiment of the invention 1.By these two photos as can be seen, the dense structure of the antiflaming magnesium alloy goods that the embodiment of the invention 1 makes, crystal boundary is clear, and impurity is few.
Embodiment 2
The first step, batching
Mass percent by component is Mg: Y: Dy=96.1: take by weighing pure magnesium, Mg-Y master alloy and Mg-Dy master alloy raw material at 0.40: 3.5, wherein, the mass percent that the Mg-Y master alloy contains Y be 29.05% all the other are Mg, the mass percent that the Mg-Dy master alloy contains Dy be 29.025% all the other are Mg, used pure magnesium is commercial commodity, and Mg-Y master alloy and Mg-Dy master alloy are available from Inner Mongol rare earth research institute;
Second step, the melting of rare earth flame resistance magnesium alloy
With embodiment 1;
In the 3rd step, be cast into the antiflaming magnesium alloy goods
With embodiment 1, the atomic percent that promptly makes component is Mg
96.1Y
0.40Dy
3.5The antiflaming magnesium alloy goods.
Embodiment 3
The first step, batching
Mass percent by component is Mg: Y: Dy=97.05: take by weighing pure magnesium, Mg-Y master alloy and Mg-Dy master alloy raw material at 0.45: 2.5, wherein, the mass percent that the Mg-Y master alloy contains Y be 29.05% all the other are Mg, the mass percent that the Mg-Dy master alloy contains Dy be 29.025% all the other are Mg, used pure magnesium is commercial commodity, and Mg-Y master alloy and Mg-Dy master alloy are available from Inner Mongol rare earth research institute;
Second step, the melting of rare earth flame resistance magnesium alloy
With embodiment 1;
In the 3rd step, be cast into the antiflaming magnesium alloy goods
With embodiment 1, the atomic percent that promptly makes component is Mg
97.05Y
0.45Dy
2.5The antiflaming magnesium alloy goods.
Embodiment 4
The first step, batching
Mass percent by component is Mg: Y: Dy=98.19: take by weighing pure magnesium, Mg-Y master alloy and Mg-Dy master alloy raw material at 0.31: 1.5, wherein, the mass percent that the Mg-Y master alloy contains Y be 29.05% all the other are Mg, the mass percent that the Mg-Dy master alloy contains Dy be 29.025% all the other are Mg, used pure magnesium is that commercial purity is that mass percent is 99.95% pure magnesium, and Mg-Y master alloy and Mg-Dy master alloy are available from Inner Mongol rare earth research institute;
Second step, the melting of rare earth flame resistance magnesium alloy
With embodiment 1;
In the 3rd step, be cast into the antiflaming magnesium alloy goods
With embodiment 1, the atomic percent that promptly makes component is Mg
98.19Y
0.31Dy
1.5The antiflaming magnesium alloy goods.
Embodiment 5
The first step, batching
Mass percent by component is Mg: Y: Dy=96.0: take by weighing pure magnesium, Mg-Y master alloy and Mg-Dy master alloy raw material at 0.50: 3.5, wherein, the mass percent that the Mg-Y master alloy contains Y be 29.05% all the other are Mg, the mass percent that the Mg-Dy master alloy contains Dy be 29.025% all the other are Mg, used pure magnesium is that commercial purity is that mass percent is 99.95% pure magnesium, and Mg-Y master alloy and Mg-Dy master alloy are available from Inner Mongol rare earth research institute;
Second step, the melting of rare earth flame resistance magnesium alloy
With embodiment 1;
In the 3rd step, be cast into the antiflaming magnesium alloy goods
With embodiment 1, the atomic percent that promptly makes component is Mg
96.0Y
0.50Dy
3.5The antiflaming magnesium alloy goods.
Make in the homodisperse process of rare earth element in the described mechanical stirring of carrying out of the foregoing description, the liquid magnesium alloy surface is steadily pure, there is no the ignition phenomenon and takes place; And the liquid level self-regeneration rapidly on liquid magnesium alloy surface when stirring, stoped the adding of outside air effectively; The liquid magnesium alloy levelling is steady during casting, does not have emerging of any Mars flicker and dense smoke.
The antiflaming magnesium alloy that above-mentioned all embodiment are made carries out flame retardant test, and the result is that its burning-point has all improved more than 200 ℃ than pure magnesium burning-point, and the mean value of burning-point has reached more than 850 ℃.In test burning-point process; when the antiflaming magnesium alloy part that above-mentioned all embodiment make has Mars to glimmer; itself self-regeneration rapidly; stoped incendiary further to carry out; further heating; after the antiflaming magnesium alloy fusing that above-mentioned all embodiment make, its surperficial oxide film toughness is all fine, has protected the liquid magnesium alloy of molten state effectively.
Claims (1)
1. rare earth flame resistance magnesium alloy, it is characterized in that: it is a magnesium yttrium dysprosium ternary antiflaming magnesium alloy, and the atomic percent of its component is Mg
96.0～98.19Y
0.31～0.5Dy
1.5～3.5
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| CN101629261B true CN101629261B (en) | 2010-12-08 |
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| CN102085387A (en) * | 2010-12-20 | 2011-06-08 | 苏州奥芮济医疗科技有限公司 | In vivo absorbable metal intervertebral fusion cage |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092671A (en) * | 2007-07-05 | 2007-12-26 | 北京有色金属研究总院 | Low cost heat-resistant magnesium alloy containing rare earth, and prepartion method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092671A (en) * | 2007-07-05 | 2007-12-26 | 北京有色金属研究总院 | Low cost heat-resistant magnesium alloy containing rare earth, and prepartion method |
Non-Patent Citations (1)
| Title |
|---|
| 王志峰等.AZ91-1.0%RE镁合金及其高温热处理研究.《铸造》.2008,第57卷(第8期),第775-779. * |
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