CN104195398A - Preparation method of magnesium-yttrium alloy - Google Patents
Preparation method of magnesium-yttrium alloy Download PDFInfo
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- CN104195398A CN104195398A CN201410463015.1A CN201410463015A CN104195398A CN 104195398 A CN104195398 A CN 104195398A CN 201410463015 A CN201410463015 A CN 201410463015A CN 104195398 A CN104195398 A CN 104195398A
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Abstract
The invention discloses a preparation method of magnesium-yttrium alloy. The preparation method comprises the following steps: taking magnesium powder and magnesium particles as raw materials of magnesium, and taking yttrium powder as a raw material of yttrium; fully mixing the magnesium powder with the yttrium powder, and pressing into blocks; putting the magnesium-yttrium blocks and the magnesium particles into a quartz tube according to the composition of the magnesium-yttrium alloy, vacuumizing the quartz tube, and sealing; vertically arranging the quartz tube, heating for melting the raw materials, after the melting process is finished, quickly cooling the quartz tube, and after liquid in the quartz tube is completely solidified, breaking the quartz tube to obtain the product-magnesium-yttrium alloy, wherein the quartz tube swings left and right along the central axis of the quartz tube in the melting process. The preparation process is simple; through combination of various conditions, no impurity elements are doped in the preparation process, so that the required amount of alloy can be accurately obtained; the yttrium content is good in controllability; the obtained magnesium-yttrium alloy is nearly free of impurities; yttrium exists in the form of Mg24Y5 and can serve as the stable raw material for preparing Mg-Zn-Y quasi-crystals; the process has a good industrialized prospect.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium-yttrium master alloy, the preparation method of magnesium-yittrium alloy that particularly a kind of impurity is few, content controllability is strong, belongs to magnesium-rare earth preparing technical field.
Background technology
Magnesium alloy is the lightest structural metallic material of applying at present, and it has high specific tenacity and specific rigidity and good castability,, has broad application prospects to loss of weight and energy-saving and cost-reducing remarkable especially in fields such as automobile, electronics, aerospace.Although magnesium alloy room-temperature property excellence, but poor resistance toheat has limited the application of magnesium alloy, the high-temperature behavior that therefore adopts variety of way to improve magnesium alloy is the key of magnesium alloy widespread use.At present except improving its resistance toheat by add the elements such as rare earth in magnesium alloy, creep property and the thermostability of utilizing accurate crystalline phase to improve magnesium alloy are also that the high-temperature behavior that an accurate crystalline phase of important research means, particularly Mg-Zn-Y strengthens Magnuminium is improved particularly evident.
But preparation Mg-Zn-Y quasicrystalline alloy requires harsher for composition and curing condition, especially the Composition Control of rare earth element y is particularly important, owing to directly adding the as easy as rolling off a log rare earth scaling loss that causes of Y in molten metal magnesium, therefore prepare in Mg-Zn-Y quasicrystalline alloy process and conventionally adopt Mg-Y master alloy form to add to reduce the scaling loss of Y.Being prepared with of current Mg-Y master alloy is several lower several:
Patent CN201210556082.9 discloses a kind of magnesium-yittrium alloy, and its raw material consists of: Y4.52-5.81%, and Nd2.21-2.58%, Ni0.01-0.03%, Cu0.015-0.023%, all the other are magnesium and impurity.The preparation method of this alloy is: above-mentioned raw materials is carried out to melting-cast-extrusion processing, to obtain final product.
Patent CN200510119121.9 discloses the method for the high moisture material electrolytic preparation rare-earth and Mg master alloy of a kind of use, the method is in fused chloride molten salt system, directly will contain the moisture material of the Yttrium trichloride of 0.56 ~ 5.4 crystal water and the height of rich lanthanum mixed chlorinated rare earth and drop into electrolytic tank electrolysis, produce in the middle of Y-Mg or ML-Mg, solved the technical barrier being difficult to high moisture material electrolytic preparation rare-earth and Mg master alloy.
Deng Wei equality has been delivered one section of fused salt electrolysis by name and has produced the article (Deng Weiping of magnesium yittrium alloy and metallic yttrium, Zeng Xingdi, pond is eastwards. and magnesium yittrium alloy and metallic yttrium are produced in fused salt electrolysis. rare earth .1997, , 18(2) .), method is: by the yttrium fluoride preparing, lithium fluoride mixture adds electrolyzer, insert negative electrode, starting the arc molten electrolyte, constantly add mixture, in the time of electrolyte solution fusing a great deal of, yttrium oxide and magnesium oxide are added in stove, after magnesium fusing, maintaining cathode end is surrounded by liquid magnesium, regulate electric current to preset value, start electrolysis, after electrolysis is complete, mention negative electrode, scoop out alloy cast ingot.
Remaining Qiu Xin etc. delivered one section of article that is called the research of yttrium magnesium codeposition in Molten Chlorides (Yu Qiuxin, Yang Qiqin, Liu Guankun. the research of yttrium magnesium codeposition in Molten Chlorides. rare metal, 1985,86: 35), at KCl-YCl
3-MgCl
2in melt, prepare the yttrium-magnesium alloy that contains yttrium 60% left and right with electrolysis co-electrodeposition method.
Not only energy consumption is larger for above-mentioned these preparation methods, and the meeting having in preparation process produces toxic gas, contaminate environment, be detrimental to health, in addition, adopt these methods to prepare in magnesium-yttrium master alloy process and inevitably can introduce impurity element as Fe, Ni, Mn etc., can not form highly purified magnesium yittrium alloy, this is also very unfavorable to prepare the accurate crystalline phase of Mg-Zn-Y with magnesium yittrium alloy.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of magnesium-yittrium alloy, the method raw material adds mode uniqueness, melting under vacuum condition, rapid solidification after melting, safe preparation process, non-environmental-pollution, in magnesium-yttrium master alloy inclusion-free of gained, alloy, constituent content controllability is strong.
The present invention is divided into two kinds of forms by magnesium and carries out melting; a part is with the form and yttrium powder mixing briquetting of magnesium powder, and another part exists with the form of magnesium grain, will after magnesium-yttrium piece and the mixing of magnesium grain, add in vacuum-packed silica tube; through melting rapid solidification, obtain magnesium-yittrium alloy.In preparation process, by the collocation that adds mode, melting and solidification mode of magnesium, yttrium has been realized, inclusion-free in alloy is sneaked into, the strong technical purpose of constituent content controllability in alloy, make purity high, the preparation of the magnesium-yittrium alloy of required component is easy to realize.
The concrete technical scheme of the present invention is as follows:
A preparation method for magnesium-yittrium alloy, is characterized in that comprising the following steps:
(1) select magnesium powder and the magnesium grain raw material as element magnesium, select the raw material of yttrium powder as Yt;
(2) magnesium powder and yttrium powder are fully mixed to briquetting;
(3), according to the composition of magnesium-yittrium alloy, above-mentioned magnesium-yttrium piece and magnesium grain are put into silica tube, then by silica tube sealed after being vacuumized;
(4) vertically place silica tube, it is heated, make the raw materials melt in silica tube, in melting process, silica tube swings along its central shaft, after melting, silica tube is placed in rapidly at the temperature of 10-20 DEG C coolingly, after the liquid in silica tube solidifies completely, breaks silica tube, products obtained therefrom is magnesium-yittrium alloy.
In magnesium yittrium alloy of the present invention, the content of yttrium can reach 20～38wt%, and surplus is magnesium, also likely with the trace impurity of introducing in raw material.All in vacuum process, carry out because of whole melting process and process of cooling, therefore in preparation process, do not have impurity and introduce, compare and existing additive method, gained alloy impurity content is few.
In the magnesium yittrium alloy that the inventive method obtains, yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist.
In aforesaid method, for magnesium, yttrium are mixed, in melting process, silica tube is vertically placed, allowed silica tube do axial wobble along its central shaft, as shown in Figure 3 always.Can ensure like this in melting process that magnesium and yttrium mix more even, the magnesium yittrium alloy crystal grain making disperses more even.The pendulum angle α of silica tube can select within the scope of 0～90 °, and pendulum angle is larger, and it is better to mix, but is no more than 90 °, preferably 60～90 °.
In above-mentioned preparation method, in step (1), selected magnesium powder and yttrium powder should be as far as possible pure, all should be more than or equal to 99.9%, and granularity is 200～700 orders, and preferably both granulometric facies are same.
In above-mentioned preparation method, in step (2), in order to be that magnesium powder and yttrium powder mix, the volume ratio of magnesium powder and yttrium powder is 1:1.
In above-mentioned preparation method, in step (2), magnesium powder and yttrium powder can adopt any existing mode to mix, and preferably adopt in the present invention following hybrid mode: in magnesium powder and yttrium powder, add dehydrated alcohol, in mortar, mix, naturally dry.
In above-mentioned preparation method, in step (2), the block density of suppressing is 70%～80%.Density reflection block porosity number.Density is too high or too low, can make the content of yttrium in gained alloy and setting content deviation become large, makes constituent content controllability step-down.
In above-mentioned preparation method, in step (2), the shape of magnesium yttrium piece can be cylindrical, can be also rectangular parallelepiped or square.Consider that silica tube waves block in process and can produce certain surging force to silica tube, therefore the preferred higher cylindrical shape of roundness degree.The size of magnesium yttrium piece does not have special requirement, and it can, according to its size of the diameter control of selected silica tube, can be made one and put into silica tube, also can make polylith.
In above-mentioned preparation method, in step (2), by after magnesium powder and yttrium briquetting, after preferably magnesium yttrium piece being dried in drying baker, add again in silica tube, remove water and dehydrated alcohol in magnesium yttrium piece, to prevent content that water and alcohol residue in magnesium yttrium piece makes yttrium in gained alloy and to set content deviation and become large.Bake out temperature is generally 100-120 DEG C, general 1h of time.
In above-mentioned preparation method, in step (3), the purity of magnesium grain is more than or equal to 99.5%, and granularity is 4～6 orders.Select the consumption of magnesium yttrium piece and magnesium grain according to the content of magnesium and yttrium in magnesium yittrium alloy, adding fashionablely, preferably magnesium grain is dispersed in around magnesium yttrium piece, so that later stage magnesium and yttrium in melting process more easily mixes.
In above-mentioned preparation method, in step (3), in the time that silica tube is vacuumized, preferably after three argon gas of filling in silica tube, vacuumize again.After vacuumizing, the vacuum tightness in silica tube is 0.1 Pa～1Pa.After vacuumizing, can adopt quartz plug to carry out sealing by fusing to silica tube.
In above-mentioned preparation method, in step (4), silica tube is put into heating installation and carry out melting, conventional is vertical tubular furnace at present, can certainly adopt other heating installations that meet melting requirement in prior art.In order to meet the requirement of silica tube maintenance axial wobble in melting process, the vertical tubular furnace that can tilt and wave in can selecting now, also can select other stoves that can meet the demands, also can stove transformation now can be tilted and be waved, satisfy the demands.
In above-mentioned preparation method, in step (4), rise to 780 DEG C～830 DEG C with the temperature rise rate of 2～8 DEG C/min raw material is carried out to melting.Melting all transfers liquid to as object by solid taking raw material, and general melting soaking time is 1-2h.
In above-mentioned preparation method, in step (4), the raw material molten solution of melting gained is put into rapidly and at the temperature of 10-20 DEG C, carried out coolingly, make the fused solution can rapid solidification.In the present invention, after preferred molten, silica tube being put into rapidly to temperature is that the cooling mode of salt solution that 10-20 DEG C, concentration are 15～25wt% is carried out rapid solidification.
The invention provides a kind of preparation method who prepares magnesium-yittrium alloy, the method preparation technology is simple, by the collocation of each condition, inclusion-free element in preparation process is mixed, can obtain more accurately the alloy of desired content, yttrium content controllability is strong, almost inclusion-free of the magnesium-yittrium alloy of gained, yttrium content is higher, and yttrium is all with Mg
24y
5form exist, and it is comparatively even to distribute, and can be used as the accurate brilliant stable raw material of preparation Mg-Zn-Y, technique industrialization prospect is good.
Brief description of the drawings
The XRD diffractogram of magnesium-yttrium master alloy that Fig. 1 is prepared according to embodiment 1;
The SEM of magnesium-yttrium master alloy that Fig. 2 is prepared according to embodiment 1.
Fig. 3 silica tube is along the swing schematic diagram of (axial wobble) of its central shaft.
Embodiment
Further set forth thinking of the present invention and advantage by specific examples below, following embodiment only plays explanation effect to the present invention, its content is not limited.In following embodiment, if no special instructions, related percentage composition is quality percentage composition.
In following embodiment, magnesium powder used, yttrium powder, magnesium grain are commercially available prod.Wherein, the purity of magnesium powder and yttrium powder is all greater than 99.9%, and granularity is 200～700 orders.The purity of magnesium grain is more than or equal to 99.5%, and granularity is 4～6 orders.
embodiment 1
Design batching according to Mg-20%Y alloy, its preparation method is:
1, Mg powder and Y powder adopted to wet-mixed evenly and naturally dry according to volume ratio 1:1, taking 200 grams of mixed powders, mixed powder is pressed into nahlock with 50MPa pressure on tabletting machine, the density of nahlock is 71.5%; Described wet-mixed method is: magnesium powder and yttrium powder are added in appropriate dehydrated alcohol, grind in platinum mix (lower same) at agate;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the magnesium grain of 521 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 1Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 780 DEG C with the temperature rise rate of 2 DEG C/min from room temperature, is then incubated 1h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 70
o, after insulation finishes, silica tube being put into temperature is the salt solution that 20 DEG C, concentration are 20wt%, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
Magnesium-the yittrium alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 19.8%, all the other are Mg.In alloy, yttrium content and theoretical content 20% are basic identical.
Fig. 1 is the XRD figure of gained alloy, as can be seen from the figure: prepared magnesium-yittrium alloy only contains α-Mg and Mg
24y
5phase, yttrium is all with Mg
24y
5form exist.
Fig. 2 is the SEM figure of gained alloy, as can be seen from the figure: white is Mg mutually
24y
5, on matrix α-Mg, distribute comparatively even.
embodiment 2
Design batching according to Mg-25%Y alloy, its preparation method is:
1, be that 1:1 adopts wet-mixed evenly and naturally dries by Mg powder and Y powder according to volume ratio, take 200 grams of mixed powders, mixed powder is pressed into nahlock with 55MPa pressure on tabletting machine, the density of nahlock is 73.1%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the magnesium grain of 376 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 0.8Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 800 DEG C with the temperature rise rate of 5 DEG C/min from room temperature, is then incubated 1.5h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 90
o, it is the salt solution that 20 DEG C, concentration are 20wt% that insulation finishes the rear temperature of rapidly silica tube being put into, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
Magnesium-the yittrium alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 24.7%, all the other are Mg.In alloy, yttrium content and theoretical content 25% are basic identical.The XRD figure of gained alloy is similar to Fig. 1, and yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist, distributed components in alloy.
embodiment 3
Design batching according to Mg-30%Y alloy, its preparation method is:
1, be that 1:1 adopts wet-mixed evenly and naturally dries by Mg powder and Y powder according to volume ratio, take 200 grams of mixed powders, mixed powder is pressed into nahlock with 55MPa pressure on tabletting machine, the density of nahlock is 73.3%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the magnesium grain of 281 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 0.5Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 820 DEG C with the temperature rise rate of 5 DEG C/min from room temperature, is then incubated 1.5h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 80
o, it is the salt solution that 20 DEG C, concentration are 20wt% that insulation finishes the rear temperature of rapidly silica tube being put into, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
Magnesium-yttrium master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 29.8%, all the other are Mg.In alloy, yttrium content and theoretical content 30% are basic identical.The XRD figure of gained alloy is similar to Fig. 1, and yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist, distributed components in alloy.
embodiment 4
Design batching according to Mg-35%Y alloy, its preparation method is:
1, be that 1:1 adopts wet-mixed evenly and naturally dries by Mg powder and Y powder according to volume ratio, take 200 grams of mixed powders, mixed powder is pressed into nahlock with 60MPa pressure on tabletting machine, the density of nahlock is 75.2%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the magnesium grain of 212 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 0.2Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 830 DEG C with the temperature rise rate of 8 DEG C/min from room temperature, is then incubated 2h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 60
o, it is the salt solution that 20 DEG C, concentration are 20wt% that insulation finishes the rear temperature of rapidly silica tube being put into, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
Magnesium-yttrium master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 34.6%, all the other are Mg.In alloy, yttrium content and theoretical content 35% are basic identical.The XRD figure of gained alloy is similar to Fig. 1, and yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist, distributed components in alloy.
embodiment 5
Design batching according to Mg-38%Y master alloy, its preparation method is:
1, be that 1:1 adopts wet-mixed evenly and naturally dries by Mg powder and Y powder according to volume ratio, take 200 grams of mixed powders, mixed powder is pressed into nahlock with 60MPa pressure on tabletting machine, the density of nahlock is 74.7%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the spherical magnesium grain of 179 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 0.1Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 830 DEG C with the temperature rise rate of 2 DEG C/min from room temperature, is then incubated 1.5h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 75
o, it is the salt solution that 10 DEG C, concentration are 15wt% that insulation finishes the rear temperature of rapidly silica tube being put into, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
Magnesium-yttrium master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 37.5%, all the other are Mg.In alloy, yttrium content and theoretical content 38% are basic identical.The XRD figure of gained alloy is similar to Fig. 1, and yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist, distributed components in alloy.
embodiment 6
Design batching according to Mg-38%Y master alloy, its preparation method is:
1, be that 1:1 adopts wet-mixed evenly and naturally dries by Mg powder and Y powder according to volume ratio, take 200 grams of mixed powders, mixed powder is pressed into nahlock with 65MPa pressure on tabletting machine, the density of nahlock is 79.2%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the spherical magnesium grain of 179 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 0.1Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 830 DEG C with the temperature rise rate of 2 DEG C/min from room temperature, is then incubated 1.5h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 70
o, it is the salt solution that 20 DEG C, concentration are 20wt% that insulation finishes the rear temperature of rapidly silica tube being put into, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
Magnesium-yttrium master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 37.6%, all the other are Mg.In alloy, yttrium content and theoretical content 38% are basic identical.The XRD figure of gained alloy is similar to Fig. 1, and yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist, distributed components in alloy.
comparative example 1
Design batching according to Mg-38%Y master alloy, its preparation method is:
1, be that 1:1 adopts wet-mixed evenly and naturally dries by Mg powder and Y powder according to volume ratio, take 200 grams of mixed powders, mixed powder is pressed into nahlock with 65MPa pressure on tabletting machine, the density of nahlock is 79.2%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, around block, disperse to add the spherical magnesium grain of 179 grams, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 0.1Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, temperature rise rate with 2 DEG C/min rises to 830 DEG C from room temperature, then be incubated 1.5h, in melting process, vertical tubular furnace waves, and it is the salt solution that 20 DEG C, concentration are 20wt% that insulation finishes the rear temperature that rapidly silica tube fallen into rapidly, and sample is carried out to rapid solidification, after completely cooling, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy.
Magnesium-yttrium master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 36.9%, all the other are Mg.There is the not Y simple substance of complete reaction in the sample central position that obtains, in sample, Y element distributes very inhomogeneous, sample center to surface and sample top to bottom all present obvious constant gradient and distribute, and institute's Mg-Y segregation that obtains is serious, is unfavorable for using in magnesium alloy smelting as master alloy.
comparative example 2
Prepare Mg-20%Y alloy according to the method for embodiment 1, different: the step of step 3 is as follows:
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 780 DEG C with the temperature rise rate of 2 DEG C/min from room temperature, is then incubated 1h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 70
o, after insulation finishes, by silica tube furnace cooling, after completely cooling, break silica tube into pieces and take out the alloy pig of preparation, be magnesium-yittrium alloy.
Magnesium-yittrium alloy component segregation of the present embodiment gained is serious, and in sample, Y element distributes very inhomogeneously, and sample top to bottom all presents obvious constant gradient and distributes, and is unfavorable for using in magnesium alloy smelting as master alloy.
comparative example 3
Design batching according to Mg-20%Y alloy, its preparation method is:
1, Mg powder and Y powder adopted to wet-mixed evenly and naturally dry according to volume ratio 1:3, taking 200 grams of mixed powders, mixed powder is pressed into nahlock with 50MPa pressure on tabletting machine, the density of nahlock is 70.1%;
2, pressed nahlock is dried and is placed in silica tube in baking oven, the content of magnesium in dispersion interpolation magnesium powder around block is supplied alloy, then after silica tube being adopted to high-purity argon gas (99.999%) filling three times, vacuumize and use quartz plug to carry out sealing by fusing to silica tube, the vacuum tightness after vacuum-sealing in silica tube is 1Pa;
3, vacuum-packed silica tube is positioned in the vertical tubular furnace that tiltable waves, intensification melting, rises to 780 DEG C with the temperature rise rate of 2 DEG C/min from room temperature, is then incubated 1h, the tube furnace in melting process that simultaneously heats up is constantly vacillated now to the left, now to the right vertically, and pendulum angle is 70
o, after insulation finishes, silica tube being fallen into rapidly to temperature is the salt solution that 20 DEG C, concentration are 20wt%, and sample is carried out to rapid solidification, breaks silica tube into pieces and take out the alloy pig of preparation after completely cooling, is magnesium-yittrium alloy.
There is component segregation in the magnesium-yittrium alloy of the present embodiment gained, sample surfaces have part Mg simple substance exist, in sample Y element distribute very inhomogeneous, be unfavorable for using in magnesium alloy smelting as master alloy.
Claims (10)
1. a preparation method for magnesium-yittrium alloy, is characterized in that comprising the following steps:
(1) select magnesium powder and the magnesium grain raw material as element magnesium, select the raw material of yttrium powder as Yt;
(2) magnesium powder and yttrium powder are fully mixed to briquetting;
(3), according to the composition of magnesium-yittrium alloy, above-mentioned magnesium-yttrium piece and magnesium grain are put into silica tube, then by silica tube sealed after being vacuumized;
(4) vertically place silica tube, it is heated, make the raw materials melt in silica tube, in melting process, silica tube swings along its central shaft, after melting, silica tube is placed in rapidly at the temperature of 10-20 DEG C coolingly, after the liquid in silica tube solidifies completely, breaks silica tube, products obtained therefrom is magnesium-yittrium alloy.
2. preparation method according to claim 1, is characterized in that: the angle that silica tube swings is up to 90 °, preferably 60～90 °.
3. preparation method according to claim 1 and 2, is characterized in that: in step (2), block density is 70%～80%.
4. preparation method according to claim 1 and 2, is characterized in that: in step (2), the volume ratio of magnesium powder and yttrium powder is 1:1.
5. according to the preparation method described in any one in claim 1-4, it is characterized in that: in step (4), the salt solution that after melting, silica tube to be put into rapidly to temperature and be 10-20 DEG C, concentration be 15～25wt% is cooling; In step (4), rise to 780 DEG C～830 DEG C with the temperature rise rate of 2～8 DEG C/min raw material is carried out to melting.
6. according to the preparation method described in any one in claim 1-5, it is characterized in that: in silica tube, magnesium grain is dispersed in around magnesium yttrium piece; Vacuum tightness in silica tube is 0.1 Pa～1Pa.
7. according to the preparation method described in any one in claim 1-6, it is characterized in that: gained magnesium-yttrium piece adds in silica tube after drying at 100-120 DEG C again.
8. according to the preparation method described in any one in claim 1-7, it is characterized in that: the quality purity of Mg powder and Y powder is all more than or equal to 99.9%, granularity is 200～700 orders; The purity of magnesium grain is more than or equal to 99.5%, and granularity is 4～6 orders.
9. according to the preparation method described in any one in claim 1-8, it is characterized in that: in magnesium-yittrium alloy, yttrium content is 20wt%～38wt%.
10. according to the preparation method described in any one in claim 1-9, it is characterized in that: in gained magnesium yittrium alloy, yttrium is with Mg
24y
5form exist, magnesium is with α-Mg and Mg
24y
5form exist.
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| CN113234978A (en) * | 2021-05-08 | 2021-08-10 | 合肥诺瓦新材料科技有限公司 | Extruded magnesium-yttrium alloy and preparation method thereof |
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| JP2002249801A (en) * | 2001-02-26 | 2002-09-06 | National Institute Of Advanced Industrial & Technology | Method for manufacturing corrosion resistant magnesium alloy and material |
| CN1683281A (en) * | 2004-04-14 | 2005-10-19 | 中国科学院电工研究所 | Process for preparing magnesium diboride superconductor |
| CN102676897A (en) * | 2012-05-17 | 2012-09-19 | 燕山大学 | Anti-corrosion magnalium base alloy and preparation method thereof |
| CN103014399A (en) * | 2012-12-31 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of enhanced magnesium-based composite material of carbon nanotubes |
| CN103898344A (en) * | 2012-12-24 | 2014-07-02 | 北京有色金属研究总院 | Preparation method of copper based diamond matrix composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002249801A (en) * | 2001-02-26 | 2002-09-06 | National Institute Of Advanced Industrial & Technology | Method for manufacturing corrosion resistant magnesium alloy and material |
| CN1683281A (en) * | 2004-04-14 | 2005-10-19 | 中国科学院电工研究所 | Process for preparing magnesium diboride superconductor |
| CN102676897A (en) * | 2012-05-17 | 2012-09-19 | 燕山大学 | Anti-corrosion magnalium base alloy and preparation method thereof |
| CN103898344A (en) * | 2012-12-24 | 2014-07-02 | 北京有色金属研究总院 | Preparation method of copper based diamond matrix composite material |
| CN103014399A (en) * | 2012-12-31 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of enhanced magnesium-based composite material of carbon nanotubes |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113234978A (en) * | 2021-05-08 | 2021-08-10 | 合肥诺瓦新材料科技有限公司 | Extruded magnesium-yttrium alloy and preparation method thereof |
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