CN1948532A - Quasi crystal phase fortified magnesium lithium alloy and its preparation method - Google Patents

Quasi crystal phase fortified magnesium lithium alloy and its preparation method Download PDF

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CN1948532A
CN1948532A CN 200610134114 CN200610134114A CN1948532A CN 1948532 A CN1948532 A CN 1948532A CN 200610134114 CN200610134114 CN 200610134114 CN 200610134114 A CN200610134114 A CN 200610134114A CN 1948532 A CN1948532 A CN 1948532A
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alloy
crystal phase
magnesium lithium
zinc
yttrium
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CN100432258C (en
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许道奎
韩恩厚
刘路
高国忠
陈荣石
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Institute of Metal Research of CAS
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Abstract

The invention relates to Mg-Li alloy with high strength and its preparation techniques. It especially relates to Mg-Li alloy strengthened by quasi-crystalline phase and its preparation techniques, which can solve problems of alloy strengthening. Mg-Li alloy with low density, high strength and good plasticity is prepared by reasonable choosing of alloy elements and introducing quasi-crystalline phase into alloy base. The alloy is two-phase alloys of Mg-Li alloy in alpha-Mg and beta-Li phase areas. Component and content of the alloy are 5.5-11.5% Li, 0.5-15% Zn, 0.1-8% Y, and the allowances are Mg, in which percent is weight proportion. The alloy is made by melting and subsequent processing of hot extrusion and its crafts are simple and convenient to operate. Properties of materials are as follows: tensile strength is sigma b=200-300MPa, yield strength is sigma 0.2=150-260MPa, elongation percentage isdelta=17-65% and density is 1.34-1.83g/cm3.

Description

A kind of quasi crystal phase fortified magnesium lithium alloy and preparation method thereof
Technical field
The present invention relates to high strength magnesium lithium alloy and technology of preparing thereof, particularly a kind of have low density, high strength, a better deformed Mg Zinc-lithium alloy material of plasticity---quasi crystal phase fortified magnesium lithium alloy and prepare the method for this alloy material.
Background technology
Magnesium alloy is as a kind of new type of metal material, has that density is low, specific tenacity and a specific rigidity advantages of higher.(density is 0.534g/cm to adopt lithium 3) carry out alloying, not only its density can be further reduced, but also the plasticity of close-packed hexagonal magnesium alloy can be increased, this makes the Mg-Li alloy at high-technology fields such as aerospace and automobiles the potential wide application prospect be arranged.For the Mg-Li alloy, when Li content was lower than 5.5%, it was organized as α-Mg sosoloid that the Li solid solution forms in the Mg lattice.When Li content is higher than 5.5wt.%, its mainly be mutually the αGu Rongti of hcp structure and bcc structure β-Li mutually, and when Li content was higher than 11.5wt.%, alloy will be fully by the β phase composite.Wherein, duplex structure (α-Mg+ β-Li) intensity and the superplasticity for alloy is useful.
The tensile mechanical properties of table 1 typical variant magnesium lithium alloy
Alloy The extruding attitude Deng passage extruding (ECAE)
Yield strength (MPa) Tensile strength (MPa) Unit elongation (%) Yield strength (MPa) Tensile strength (MPa) Unit elongation (%)
Mg-11%Li-1%Zn Mg-9%Li-1%Zn Mg-9%Li-1%Zn-0.2%Mn Mg-9%Li-1%Zn-1%Al-0.2%Mn Mg-9%Li-1%Zn-3%Al-0.2%Mn Mg-3.3%Li 96 100 90 105 110 69 133 141 130 150 161 160 60 56 70 60 50 18 150 160 140 145 130 113 175 182 165 180 180 200 35 31 22 24 27 33
In recent years, document (Mater.Lett. (material news flash) 60 (2006) 3272) and (Scr.Mater. (material wall bulletin) 51 (2004) 1057) mainly lay particular emphasis on the intensity that following two kinds of schedule of reinforcements improve the Mg-Li alloy: 1) by adding alloy element Al, Zn and Ca strengthen.2) carrying out big viscous deformation comes the microtexture of refinement alloy to strengthen.The related data that table 1 is reported for above-mentioned document.In addition, document (Mater.Lett. (material news flash) 60 (2006) 1863) has been reported 5wt%Al 2The tensile strength of Y/Mg-Li matrix material also only is 189MPa.As can be seen, be difficult to make tensile strength of alloys (UTS) to surpass 200MPa by above three kinds of methods, this has limited the application of Mg-Li alloy in the engineering field greatly.Therefore, for mechanical property and its range of application of expansion of further improving magnesium lithium alloy, proposing a kind of new enhancement method is present problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of quasi crystal phase fortified magnesium lithium alloy and preparation method thereof, solve problems such as magnesium lithium alloy reinforcement, by the choose reasonable alloying element, accurate crystalline phase is incorporated in the magnesium lithium alloy matrix, prepared have low density, high strength, the better Mg-Li alloy of plasticity.
Technical scheme of the present invention is:
Aluminum magnesium containing alloy materials of the present invention is a quasi crystal phase fortified magnesium lithium alloy, is the two-phase magnesium lithium alloy of Mg-Li alloy in α-Mg and β-Li two-phase region, and its component and content thereof are: lithium (Li) content is 5.5~11.5%; Zinc (Zn) content is 0.5~15%; Yttrium (Y) content be 0.1~8% and the magnesium (Mg) of surplus form, all percentage ratios are mass percent; The introducing of accurate crystalline phase and zinc, yttrium content are relevant closely, and the weight ratio of zinc and yttrium (Zn/Y) is 4.5~8.
Magnesium lithium alloy material of the present invention: its tensile strength is σ b=200~300MPa, yield strength is σ 0.2=150~260MPa, unit elongation are δ=17~65%, and density is 1.34~1.83g/cm 3
The most important discovery of the present invention is: by choosing certain zinc yttrium than (Zn/Y=4.5~8), accurate crystalline phase is incorporated in the matrix of aluminum magnesium containing alloy materials, makes alloy obtain higher intensity and keeping plasticity preferably.
Strengthening mechanism of the present invention is mainly: the high rigidity that accurate crystalline phase has, low interfacial energy, have characteristics such as coherence relation with matrix, can effectively strengthen aluminum magnesium containing alloy materials.Alloying constituent of the present invention is to determine like this:
Lithium of the present invention (Li) content is 5.5~11.5%, have higher intensity owing to be in the magnesium lithium alloy of α-Mg and β-Li two-phase region, so the design of lithium content of the present invention is the magnesium lithium alloy that will obtain to be in α-Mg and β-Li two-phase region.
Zinc of the present invention (Zn) and yttrium (Y) content are respectively 0.5~15% and 0.1~8%, because the introducing and the zinc of accurate crystalline phase, yttrium content is relevant closely.When the weight ratio (Zn/Y) of zinc and yttrium is 4.5~8, zinc and yttrium will be present in the alloy substrate with accurate crystalline phase form.Therefore, the design of zinc and yttrium content is fully to guarantee accurate crystalline phase is incorporated in the alloy substrate among the present invention, reaches the purpose of reinforced alloys.
The preparation method of quasi crystal phase fortified magnesium lithium alloy of the present invention comprises and introduce accurate crystalline phase and follow-up hot extrusion processing in alloy substrate.The concrete steps of its concrete metallurgy and foundry and subsequent thermal extrusion processing process are as follows:
1) oven dry and preheating: the bake out temperature of conventional auxiliary material (covering/refining agent) is 12~180 ℃; The preheating temperature of various batchings and casting die is 150~300 ℃; Common tool (agitator, sludge ladle, bell cover, casting with scoop etc.) cleans and preheating in 700~740 ℃ molten states washing flux.
2) fusing of magnesium ingot: 720~740 ℃ of design temperatures, heat up; When crucible was preheated to garnet (400~500 ℃), residue in the cleaning crucible fed CO 2The air of gas displacement crucible inside sprinkles one deck insulating covering agent equably at crucible inwall and bottom then; The magnesium ingot that adds preheating, and on furnace charge, sprinkle one deck insulating covering agent; The insulating covering agent consumption accounts for 0.1~1.0% of charging weight in this process; Continue to heat up.
3) Pei Liao adding: when the magnesium melt temperature reaches 750~760 ℃, under the insulating covering agent protection, add various preheatings good magnesium yttrium master alloy (Mg-24%Y) and spelter according to batching fusing point order from high to low; Batching was stirred 4~6 minutes, so that composition is even after all melting; Then, remove surperficial slag, bath surface spreads with insulating covering agent.Powered-down treats that temperature reduces to 730~740 ℃, and opening power adds Li, fully stirs its fusing (is added LiCl and LiF insulating covering agent, and logical CO in this process 2Or air and SF 6Shielding gas, per-cent by volume is at 99~99.5%CO 2Or air+0.3~1%SF 6); The add-on of insulating covering agent is not burnt with bath surface and is as the criterion in this operation.
4) refining of melt: when treating that temperature is 720~730 ℃, stirred melt 7~10 minutes, melt is rolled from bottom to top, must not splash, and constantly spread on the crest of melt with refining agent (LiBr), its consumption is 0.5~2.5% of a furnace charge gross weight.
5) insulation of melt is left standstill: after refining finishes, remove the slag that alloy liquid surface, sidewall of crucible etc. are located, per-cent by volume is at 99~99.5% air (or CO 2)+0.3~1%SF 6Draw slag under mixed gas protected, bath surface spreads with insulating covering agent then, and consumption does not burn with bath surface and is as the criterion; Melt is warming up to 760~780 ℃, and insulation was left standstill 20~30 minutes.
6) cast molding operation: melt is cooled to 750~760 ℃, and (per-cent by volume is at 99~99.5%CO at the sulphur of 0.6: 1~1.4: 1 (weight ratio) and boric acid mixed powder and/or mixed gas 2Or air+0.3~1%SF 6) protection under cast.
7) extrusion molding operation: ingot casting after the homogenizing of carrying out under 350~400 ℃ 10~16 hours is handled, is carried out peeling.Is to carry out deformation processing under 180~200 ℃ to become goods with the ingot casting after the peeling in temperature.
Characteristics of the present invention are:
1, the present invention is incorporated into accurate crystalline phase in the magnesium lithium alloy matrix than (Zn/Y) by zinc yttrium in the control alloying element.
2, the present invention adopt that the inventive method has obtained to have low density, high strength, the better two-phase magnesium lithium alloy of plasticity, what be particularly suitable for lightweight, high-strength, high-ductility uses the material demand.
3, complete processing of the present invention is simple, convenient.
Description of drawings
The X-ray diffracting spectrum of three kinds of magnesium lithium alloys of Fig. 1 (embodiment 1, embodiment 2, embodiment 3).
The stereoscan photograph of the main phase of three kinds of magnesium lithium alloys of Fig. 2 (embodiment 1, embodiment 2, embodiment 3).
Mechanical property under the room temperature of three kinds of magnesium lithium alloys of Fig. 3 (embodiment 1, embodiment 2, embodiment 3).
Embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
I), alloy composition
Each element by 15 kilograms of alleged taking-ups of aluminum magnesium containing alloy materials of following proportioning configuration is: the magnesium (Mg) of lithium (Li) 1200 grams, zinc (Zn) 480 grams, magnesium yttrium master alloy (Mg-24%Y) 375 grams and surplus.By weight percentage, alloying constituent is Mg-8%Li-3.2Zn-0.6Y.
II), alloy smelting and casting
The smelting of alloy is carried out in the crucible of one 15 kg capacity and resistance furnace.Crucible and mold and pattern for casting tool adopt low-carbon steel material.Be example with embodiment 1 below, elaborate the smelting and the casting technique of alloy.
1) setting the crucible target temperature is 720 ℃, begins heating; Then various batchings such as pure magnesium, pure zinc, magnesium yttrium master alloy, pure lithium are placed on and are preheated to 150 ℃ in the baking oven, the insulating covering agent (LiCl and LiF are by carrying out weight proportion at 3: 1) that will account for purpose alloy gross weight 2% is simultaneously put into baking oven and is toasted; Casting is preheated to 300 ℃ with mould in other box-type furnace.
2) when crucible is warming up to 400 ℃, feed CO 2Gas carries out gas displacement to crucible, add about 1/2 the insulating covering agent that has toasted then in crucible bottom, again after the pure magnesium batching that preheating is good put into crucible.
3) after fusing of etc. pure magnesium batching and crucible temperature are stabilized in 750 ℃, add the magnesium yttrium master alloy and the pure zinc of preheating from high to low successively according to fusing point, melt carried out stir about 6 minutes then; In this process, take the circumstances into consideration to add the remaining insulating covering agent that has toasted, do not fire with the surface and be as the criterion.
4) treat that crucible temperature is reduced to 730 ℃ after, add Li and stir its fusing, in this process, add LiCl and LiF insulating covering agent and logical CO 2Or air and SF 6Mixed gas is protected, and the add-on of LiCl and LiF insulating covering agent is 0.6% of a charging weight; Per-cent by volume, mixed gas is at 99~99.5% air (or CO 2)+0.3~1%SF 6
When 5) treating that crucible temperature is 730 ℃, melt is carried out refining, stirred melt 10 minutes, melt is rolled from bottom to top, must not splash, and constantly in that (the melt crest refers to when stirring melt, the melt caused liquid fluctuating that rolls from bottom to top on the crest of melt, the larger part that wherein fluctuates is the melt crest location) to spread with refining agent (LiBr), the refining agent add-on is 2% of a furnace charge gross weight.
6) after refining finishes, remove the slag that alloy liquid surface, sidewall of crucible etc. are located, bath surface spreads with insulating covering agent then, and consumption does not burn with bath surface and is as the criterion; After crucible temperature was stabilized in 770 ℃, melt left standstill 20 minutes, and per-cent by volume is at 99~99.5% air (or CO 2)+0.3~1%SF 6Draw slag under mixed gas protected;
7) draw slag and finish after, keep crucible temperature and be stabilized in 750 ℃, per-cent by volume is at 99~99.5% air (or CO 2)+0.3~1%SF 6Mixed gas protected cast molding down.
III), hot extrusion processing
1) homogenizing of the ingot casting after the peeling being carried out under 400 ℃ 12 hours is handled.
2) with the ingot casting peeling.
3) ingot casting after the homogenizing processing is carried out deformation processing under 200 ℃ and become goods.
IV), microtexture characterizes
Its preparation process of the sample of structure observation is as follows: adopt No. 1000 silicon carbide silicon carbide papers to polish the surface; Adopt the mechanical polishing of oil base diamond paste then; Main in the alloy is α-Mg, β-Li, LiMgZn and Mg through the X-ray diffraction analysis 3Zn 6Y (accurate crystalline phase I-phase), corresponding X-ray spectra is listed on the accompanying drawing 1; Can determine the mainly distribution of phase in the alloy on the scanning electron microscope (Philips XL30 ESEM-FEG/EDAX) of spectral apparatus by being furnished with, scan electric brilliant photo accordingly and be listed on the accompanying drawing 2 (a).
V), Mechanics Performance Testing
Alloy at room temperature mechanics tensile property sample prepares with reference to Chinese national standard GB 228-76.The stretching sample is the pole shape, and its axis direction is parallel to the vertical of material, and the sample sl. is 25mm, and diameter is 5mm.The strain rate of tension test is 1 * 10 -3s -1Tension test is carried out on MTS (858.01M) pull and torsion test machine.The tensile strength of the material of this aluminum magnesium containing alloy is 222MPa, and yield strength is 150MPa, and unit elongation is δ=30.7%, and density is 1.41g/cm 3, corresponding stress strain curve is listed on the sequence number 1 of accompanying drawing 3.
Embodiment 2
I), alloy composition
Each element by 15 kilograms of alleged taking-ups of aluminum magnesium containing alloy materials of following proportioning configuration is: the magnesium (Mg) of lithium (Li) 1200 grams, zinc (Zn) 975 grams, magnesium yttrium master alloy (Mg-24%Y) 750 grams and surplus.By weight percentage, alloying constituent is Mg-8%Li-6.5Zn-1.2Y.
II), alloy smelting and casting
The smelting of reference example 1 and casting.Difference is: both zinc (Zn) is different with yttrium (Y) content.
III), hot extrusion processing
The extrusion process of reference example 1.
IV), microtexture characterizes
The microtexture of reference example 1 characterizes.Mainly be α-Mg, β-Li, LiMgZn, Mg mutually in the alloy 3Zn 6Y (accurate crystalline phase I-phase) and Mg 3Zn 3Y (W-phase), corresponding X-ray spectra is listed on the accompanying drawing 1; Compare with embodiment 1 interalloy, the quantity of the accurate crystalline phase I-phase in this alloy obviously increases, and scans electric brilliant photo accordingly and is listed on the accompanying drawing 2 (b).
V), Mechanics Performance Testing
The Mechanics Performance Testing of reference example 1.The tensile strength of the material of this aluminum magnesium containing alloy is 239MPa, and yield strength is 160MPa, and unit elongation is δ=20.4%, and density is 1.52g/cm 3, corresponding stress strain curve is listed on the sequence number 2 of accompanying drawing 3.
Embodiment 3
I), alloy composition
Each element by 15 kilograms of alleged taking-ups of aluminum magnesium containing alloy materials of following proportioning configuration is: the magnesium (Mg) of lithium (Li) 1200 grams, zinc (Zn) 1620 grams, magnesium yttrium master alloy (Mg-24%Y) 1187 grams and surplus.By weight percentage, alloying constituent is Mg-8%Li-10.8Zn-1.9Y.
II), alloy smelting and casting
The smelting of reference example 1 and casting.Difference is: both zinc (Zn) is different with yttrium (Y) content.
III), hot extrusion processing
The extrusion process of reference example 1.
Iv), microtexture characterizes
The microtexture of reference example 1 characterizes.Mainly be α-Mg, β-Li, LiMgZn, Mg mutually in the alloy 3Zn 6Y (accurate crystalline phase I-phase) and Mg 3Zn 3Y (W-phase), corresponding X-ray spectra is listed on the accompanying drawing 1; With the alloy phase ratio among embodiment 1 and the embodiment 2, in this alloy not only the quantity of accurate crystalline phase I-phase obviously increase and W-phase (cube phase Mg 3Zn 3Y) also begin to occur, scan electric brilliant photo accordingly and be listed on the accompanying drawing 2 (c).
V), Mechanics Performance Testing
The Mechanics Performance Testing of reference example 1.The tensile strength of the material of this aluminum magnesium containing alloy is 247MPa, and yield strength is 166MPa, and unit elongation is δ=17.1%, and density is 1.72g/cm 3, corresponding stress strain curve is listed on the sequence number 3 of accompanying drawing 3.

Claims (9)

1, a kind of quasi crystal phase fortified magnesium lithium alloy is characterized in that: the Mg-Li alloy is that its component and content thereof are at the two-phase magnesium lithium alloy of α-Mg and β-Li two-phase region: lithium content is 5.5~11.5%; Zinc content is 0.5~15%; Yttrium content is 0.1~8%; Mg content is the balance surplus.
2, according to the described quasi crystal phase fortified magnesium lithium alloy of claim 1, it is characterized in that: the weight ratio Zn/Y of zinc and yttrium is 4.5~8.
3, according to the described quasi crystal phase fortified magnesium lithium alloy of claim 1, it is characterized in that: yttrium content preferable range is 0.5~1.5% in the alloy; Zinc content preferable range is 2.5~8%.
4, according to the described quasi crystal phase fortified magnesium lithium alloy of claim 1, it is characterized in that: tensile strength of alloys is σ b=200~300MPa; The yield strength of alloy is σ 0.2=150~260MPa; The unit elongation of alloy is δ=17~65%; The density of alloy is 1.34~1.83g/cm 3
5,, it is characterized in that alloy melting and subsequent thermal extrusion processing deformation process are as follows according to the preparation method of the described quasi crystal phase fortified magnesium lithium alloy of claim 1:
1) by zinc yttrium weight ratio Zn/Y=4.5~8 than taking by weighing out alloying element zinc and yttrium;
2) when temperature is 720~740 ℃, add the pure magnesium of alloy raw material;
2) when temperature is 750~760 ℃, add alloying element zinc and magnesium yttrium master alloy Mg-24% Y
3) when temperature is reduced to 730~740 ℃, add the alloying element lithium;
4) when temperature is 720~730 ℃, alloy is carried out refining;
5) be 750~760 ℃ in temperature, cast;
6) homogenizing of the ingot casting after the peeling being carried out under 350~400 ℃ 10~16 hours is handled;
7) with the ingot casting peeling;
8) ingot casting after the homogenizing processing is carried out deformation processing under 180~200 ℃ and become goods.
6, according to the preparation method of the described quasi crystal phase fortified magnesium lithium alloy of claim 5, it is characterized in that: when the addition element lithium, adopt LiCl and LiF insulating covering agent, and logical CO 2Or air and SF 6Mixed gas is protected, and the weight ratio of LiCl and LiF is (3: 1)~(4: 1), and the weight of LiCl and LiF accounts for 2~4% of alloy gross weight; Per-cent by volume, mixed gas is 99~99.5%CO 2Or air and 0.3~1%SF 6Mix.
7, according to the preparation method of the described quasi crystal phase fortified magnesium lithium alloy of claim 5, it is characterized in that: in the refining process, spread refining agent LiBr on the crest of melt alloy is carried out refining, consumption is 0.5~2.5% of a furnace charge gross weight.
8, according to the preparation method of the described quasi crystal phase fortified magnesium lithium alloy of claim 5; it is characterized in that: when casting; protect with 0.6: 1~1.4: 1 sulphur of weight ratio and boric acid mixed powder and/or mixed gas; the add-on of sulphur and boric acid accounts for 0.5~1% of alloy gross weight; per-cent by volume, mixed gas is 99~99.5%CO 2Or air and 0.3~1%SF 6Mix.
9, according to the preparation method of the described quasi crystal phase fortified magnesium lithium alloy of claim 5, it is characterized in that: after refining finished, bath surface spread with insulating covering agent, and after crucible temperature was stabilized in 760-780 ℃, melt left standstill 20~30 minutes; Then, per-cent by volume is at 99~99.5% air or CO 2With 0.3~1%SF 6Draw slag under mixed gas protected.
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