CN104195398B - A kind of preparation method of magnesium-yittrium alloy - Google Patents
A kind of preparation method of magnesium-yittrium alloy Download PDFInfo
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- CN104195398B CN104195398B CN201410463015.1A CN201410463015A CN104195398B CN 104195398 B CN104195398 B CN 104195398B CN 201410463015 A CN201410463015 A CN 201410463015A CN 104195398 B CN104195398 B CN 104195398B
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Abstract
The invention discloses a kind of preparation method of magnesium-yittrium alloy, step comprises: using magnesium powder and magnesium grain as the raw material of element magnesium, using yttrium powder as the raw material of Yt; Magnesium powder and yttrium powder are fully mixed, briquetting; According to the composition of magnesium-yittrium alloy, magnesium-yttrium block and magnesium grain are put into silica tube, by silica tube sealed after being vacuumized; Vertical placement silica tube, heating makes raw materials melt, and in melting process, silica tube swings along its central shaft, is cooled rapidly by silica tube after melting, after the liquid in silica tube solidifies completely, break silica tube, and products obtained therefrom is magnesium-yittrium alloy.Preparation technology of the present invention is simple, by the collocation of each condition, inclusion-free element in preparation process is mixed, can obtain the alloy of desired content more accurately, and yttrium content controllability is strong, and magnesium-yittrium alloy almost inclusion-free of gained, yttrium is all with Mg
24y
5form exist, can be used as the stable raw material that preparation Mg-Zn-Y is accurate brilliant, technique industrialization prospect is good.
Description
Technical field
The present invention relates to the preparation method of a kind 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 at present application, and it has high specific tenacity and specific rigidity and excellent castability, in fields such as automobile, electronics, aerospace to loss of weight and energy-saving and cost-reducing remarkable especially, has broad application prospects.Although magnesium alloy room-temperature property is excellent, but poor resistance toheat limits the application of magnesium alloy, therefore adopt the key that the high-temperature behavior improving magnesium alloy is in various manners magnesium alloy widespread use.At present except improving except its resistance toheat by adding the elements such as rare earth in the magnesium alloy, utilizing Icosahedral phases to improve the creep property of magnesium alloy and thermostability is also that the high-temperature behavior that an important research means, particularly Mg-Zn-Y Icosahedral phases 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 in molten metal magnesium, Y is as easy as rolling off a log causes rare earth scaling loss, therefore prepares in Mg-Zn-Y quasicrystalline alloy process and usually adopts Mg-Y master alloy form to add the scaling loss reducing Y.The preparation of current Mg-Y master alloy has several lower several:
Patent CN201210556082.9 discloses a kind of magnesium-yittrium alloy, and its raw material consists of: Y4.52-5.81%, Nd2.21-2.58%, Ni0.01-0.03%, Cu0.015-0.023%, and all the other are magnesium and impurity.The preparation method of this alloy is: above-mentioned raw materials is carried out melting-cast-extrusion processing, to obtain final product.
Patent CN200510119121.9 discloses a kind of method of High water cut material electrolytic preparation rare-earth and Mg master alloy, the method is in fused chloride molten salt system, directly the High water cut material of the Yttrium trichloride containing 0.56 ~ 5.4 crystal water and rich lanthanum mixed chlorinated rare earth is dropped into electrolytic tank electrolysis, produce in the middle of Y-Mg or ML-Mg, solve the technical barrier be difficult to High water cut material electrolytic preparation rare-earth and Mg master alloy.
Deng Wei equality has delivered the article (Deng Weiping that magnesium yittrium alloy and metallic yttrium are produced in one section of fused salt electrolysis by name, 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 prepared, lithium fluoride mixture adds electrolyzer, insert negative electrode, starting the arc molten electrolyte, constantly add mixture, when electrolyte solution fusing a great deal of, yttrium oxide and magnesium oxide are added in stove, after magnesium fusing, maintain cathode end to be surrounded by liquid magnesium, regulate electric current to preset value, start electrolysis, negative electrode is mentioned after electrolysis is complete, scoop out alloy cast ingot.
Remaining Qiu Xin etc. delivered one section of article being 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 containing yttrium about 60% with electrolysis co-electrodeposition method.
Not only energy consumption is larger for these preparation methods above-mentioned, and the meeting had 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 introduce impurity element as Fe, Ni, Mn etc., can not form highly purified magnesium yittrium alloy, this is also very unfavorable to preparing Mg-Zn-Y Icosahedral phases 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 feed postition is unique, melting under vacuum, rapid solidification after melting, safe preparation process, non-environmental-pollution, in the magnesium-yttrium master alloy inclusion-free of gained, alloy, constituent content controllability is strong.
Magnesium is divided into two kinds of forms and carries out melting by the present invention; a part is with the form of magnesium powder and yttrium powder mixing briquetting, and another part exists with the form of magnesium grain, will add in vacuum-packed silica tube after magnesium-yttrium block and the mixing of magnesium grain; through melting rapid solidification, obtain magnesium-yittrium alloy.In preparation process, achieve that inclusion-free in alloy is mixed into by the collocation of the feed postition to magnesium, yttrium, melting and solidification mode, constituent content controllability is strong in alloy technical purpose, 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 magnesium grain as the raw material of element magnesium, select yttrium powder as the raw material of Yt;
(2) magnesium powder and yttrium powder are fully mixed, briquetting;
(3) according to the composition of magnesium-yittrium alloy, above-mentioned magnesium-yttrium block and magnesium grain are put into silica tube, then by silica tube sealed after being vacuumized;
(4) vertically silica tube is placed, it is heated, make the raw materials melt in silica tube, in melting process, silica tube swings along its central shaft, cool under silica tube being placed in rapidly after melting the temperature of 10-20 DEG C, after the liquid in silica tube solidifies completely, break 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 introduced in raw material.Because whole melting process and process of cooling are all carried out in vacuum process, therefore do not have impurity in preparation process 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, in order to make magnesium, yttrium mixes, and vertically placed by silica tube, allow silica tube do axial wobble along its central shaft, as shown in Figure 3 always in melting process.Can ensure that in melting process, magnesium and yttrium mix more even like this, obtained magnesium yittrium alloy grain dispersion is 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, the magnesium powder selected in step (1) 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 following hybrid mode in the present invention: in magnesium powder and yttrium powder, add dehydrated alcohol, mix, naturally dry in mortar.
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, the content of yttrium in gained alloy can be made to become greatly with setting content deviation, make constituent content controllability step-down.
In above-mentioned preparation method, in step (2), the shape of magnesium yttrium block can be cylindrical, also can be rectangular parallelepiped or square.Consider that in silica tube rocking process, block can produce certain surging force to silica tube, the cylindrical shape that therefore preferably roundness degree is higher.The not special requirement of size of magnesium yttrium block, it according to its size of the diameter control of selected silica tube, can be made one piece and put into silica tube, also can make polylith.
In above-mentioned preparation method, in step (2), after magnesium powder and yttrium briquetting, add again in silica tube after preferably magnesium yttrium block being dried in drying baker, water in removing magnesium yttrium block and dehydrated alcohol, make the content of yttrium in gained alloy become large with setting content deviation to prevent water and alcohol residue in magnesium yttrium block.Bake out temperature is generally 100-120 DEG C, time general 1h.
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 block and magnesium grain according to the content of magnesium and yttrium in magnesium yittrium alloy, adding fashionable, preferably magnesium grain is being dispersed in around magnesium yttrium block, more easily mixes to make later stage magnesium and yttrium in melting process.
In above-mentioned preparation method, in step (3), when vacuumizing silica tube, preferably vacuumize again after three argon gas of filling in silica tube.After vacuumizing, the vacuum tightness in silica tube is 0.1Pa ~ 1Pa.After vacuumizing, quartz plug can be adopted 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 in prior art other heating installations meeting melting requirement.The requirement of axial wobble is kept in order to meet silica tube in melting process, can select can tilt now the vertical tubular furnace waved, also can select other stoves that can meet the demands, also can carry out transformation to stove now and can tilt and wave, 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 and melting is carried out to raw material.Melting all transfers to for the purpose of liquid by solid by raw material, and general melting soaking time is 1-2h.
In above-mentioned preparation method, in step (4), cool under the raw material molten solution of melting gained being put into rapidly the temperature of 10-20 DEG C, enable fused solution rapid solidification.In the present invention, after preferred molten, silica tube is put into rapidly the mode that temperature is 10-20 DEG C, concentration is 15 ~ 25wt% salt solution cools and carry out rapid solidification.
The invention provides a kind of preparation method preparing magnesium-yittrium alloy, the method preparation technology is simple, by the collocation of each condition, inclusion-free element in preparation process is mixed, the alloy of desired content can be obtained more accurately, yttrium content controllability is strong, magnesium-yittrium alloy almost inclusion-free of gained, yttrium content is higher, and yttrium is all with Mg
24y
5form exist, and distribution is comparatively even, and can be used as the accurate brilliant stable raw material of preparation Mg-Zn-Y, technique industrialization prospect is good.
Accompanying drawing explanation
The XRD diffractogram of the magnesium that Fig. 1 is prepared according to embodiment 1-yttrium master alloy;
The SEM of the magnesium that Fig. 2 is prepared according to embodiment 1-yttrium master alloy.
Fig. 3 silica tube swings along its central shaft the schematic diagram of (axial wobble).
Embodiment
Set forth thinking of the present invention and advantage further below by way of specific examples, following embodiment only plays explanation effect to the present invention, does not limit its content.In following embodiment, if no special instructions, involved percentage composition is mass percentage.
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
Carry out design batching according to Mg-20%Y alloy, its preparation method is:
1, adopt wet-mixed evenly according to volume ratio 1:1 in Mg powder and Y powder and naturally dry, take mixed powder 200 grams, mixed powder is pressed into nahlock with 50MPa pressure on tabletting machine, the density of nahlock is 71.5%; Described wet-mixed method is: add in appropriate dehydrated alcohol by magnesium powder and yttrium powder, grinds in platinum mix (lower same) at agate;
2, pressed nahlock is dried in an oven be placed in silica tube, the magnesium grain of interpolation 521 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 70
o, after insulation terminates silica tube put into that temperature is 20 DEG C, concentration is the salt solution of 20wt%, rapid solidification carried out to sample, after cooling completely, breaks the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy.
Magnesium-the yittrium alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 19.8%, and all the other are Mg.In alloy, yttrium content is substantially identical with theoretical content 20%.
Fig. 1 is the XRD figure of gained alloy, as can be seen from the figure: prepared magnesium-yittrium alloy is only containing 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, matrix α-Mg distributes comparatively even.
embodiment 2
Carry out 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 mixed powder 200 grams, mixed powder is pressed into nahlock with 55MPa pressure on tabletting machine, the density of nahlock is 73.1%;
2, pressed nahlock is dried in an oven be placed in silica tube, the magnesium grain of interpolation 376 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 90
o, insulation terminates rapidly silica tube to be put into that temperature is 20 DEG C, concentration is the salt solution of 20wt% afterwards, carries out rapid solidification, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy after cooling completely sample.
Magnesium-the yittrium alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 24.7%, and all the other are Mg.In alloy, yttrium content is substantially identical with theoretical content 25%.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
Carry out 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 mixed powder 200 grams, mixed powder is pressed into nahlock with 55MPa pressure on tabletting machine, the density of nahlock is 73.3%;
2, pressed nahlock is dried in an oven be placed in silica tube, the magnesium grain of interpolation 281 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 80
o, insulation terminates rapidly silica tube to be put into that temperature is 20 DEG C, concentration is the salt solution of 20wt% afterwards, carries out rapid solidification, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy after cooling completely sample.
Magnesium-yttrium the master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 29.8%, and all the other are Mg.In alloy, yttrium content is substantially identical with theoretical content 30%.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
Carry out 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 mixed powder 200 grams, mixed powder is pressed into nahlock with 60MPa pressure on tabletting machine, the density of nahlock is 75.2%;
2, pressed nahlock is dried in an oven be placed in silica tube, the magnesium grain of interpolation 212 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 60
o, insulation terminates rapidly silica tube to be put into that temperature is 20 DEG C, concentration is the salt solution of 20wt% afterwards, carries out rapid solidification, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy after cooling completely sample.
Magnesium-yttrium the master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 34.6%, and all the other are Mg.In alloy, yttrium content is substantially identical with theoretical content 35%.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
Carry out 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 mixed powder 200 grams, mixed powder is pressed into nahlock with 60MPa pressure on tabletting machine, the density of nahlock is 74.7%;
2, pressed nahlock is dried in an oven be placed in silica tube, the spherical magnesium grain of interpolation 179 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 75
o, insulation terminates rapidly silica tube to be put into that temperature is 10 DEG C, concentration is the salt solution of 15wt% afterwards, carries out rapid solidification, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy after cooling completely sample.
Magnesium-yttrium the master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 37.5%, and all the other are Mg.In alloy, yttrium content is substantially identical with theoretical content 38%.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
Carry out 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 mixed powder 200 grams, mixed powder is pressed into nahlock with 65MPa pressure on tabletting machine, the density of nahlock is 79.2%;
2, pressed nahlock is dried in an oven be placed in silica tube, the spherical magnesium grain of interpolation 179 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 70
o, insulation terminates rapidly silica tube to be put into that temperature is 20 DEG C, concentration is the salt solution of 20wt% afterwards, carries out rapid solidification, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy after cooling completely sample.
Magnesium-yttrium the master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 37.6%, and all the other are Mg.In alloy, yttrium content is substantially identical with theoretical content 38%.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
Carry out 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 mixed powder 200 grams, mixed powder is pressed into nahlock with 65MPa pressure on tabletting machine, the density of nahlock is 79.2%;
2, pressed nahlock is dried in an oven be placed in silica tube, the spherical magnesium grain of interpolation 179 grams is disperseed around block, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, 830 DEG C are risen to from room temperature with the temperature rise rate of 2 DEG C/min, then 1.5h is incubated, in melting process, vertical tubular furnace waves, and insulation terminates rapidly silica tube to be fallen into rapidly that temperature is 20 DEG C, concentration is the salt solution of 20wt% afterwards, carries out rapid solidification to sample, after cooling completely, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy.
Magnesium-yttrium the master alloy of the present embodiment gained, utilizing direct-reading spectrometer to record Y content is 36.9%, and all the other are Mg.Obtain the Y simple substance that non-complete reaction appears in sample central position, in sample, Y element distribution is very uneven, sample center to surface and sample top to bottom all presents the distribution of obvious constant gradient, and institute's Mg-Y segregation that obtains is serious, is unfavorable for using in magnesium alloy smelting as master alloy.
comparative example 2
Mg-20%Y alloy is prepared according to the method for embodiment 1, unlike: 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 70
o, by silica tube furnace cooling after insulation terminates, after cooling completely, break the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy.
Magnesium-yittrium alloy the component segregation of the present embodiment gained is serious, and in sample, Y element distribution is very uneven, and sample top to bottom all presents the distribution of obvious constant gradient, is unfavorable for using in magnesium alloy smelting as master alloy.
comparative example 3
Carry out design batching according to Mg-20%Y alloy, its preparation method is:
1, adopt wet-mixed evenly according to volume ratio 1:3 in Mg powder and Y powder and naturally dry, take mixed powder 200 grams, mixed powder is pressed into nahlock with 50MPa pressure on tabletting machine, the density of nahlock is 70.1%;
2, pressed nahlock is dried in an oven be placed in silica tube, around block, the content that magnesium powder supplies magnesium in alloy is added in dispersion, then vacuumize after silica tube being adopted high-purity argon gas (99.999%) filling three times 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, in intensification melting process, tube furnace is constantly vacillated now to the left, now to the right vertically simultaneously, and pendulum angle is 70
o, after insulation terminates silica tube fallen into rapidly that temperature is 20 DEG C, concentration is the salt solution of 20wt%, rapid solidification carried out to sample, after cooling completely, breaks the alloy pig that silica tube takes out preparation into pieces, be magnesium-yittrium alloy.
There is component segregation in the magnesium-yittrium alloy of the present embodiment gained, sample surfaces has part Mg simple substance to exist, and in sample, Y element distribution is very uneven, is unfavorable for using in magnesium alloy smelting as master alloy.
Claims (9)
1. a preparation method for magnesium-yittrium alloy, is characterized in that comprising the following steps:
(1) select magnesium powder and magnesium grain as the raw material of element magnesium, select yttrium powder as the raw material of Yt;
(2) magnesium powder and yttrium powder are fully mixed, briquetting;
(3) according to the composition of magnesium-yittrium alloy, above-mentioned magnesium-yttrium block and magnesium grain are put into silica tube, then by silica tube sealed after being vacuumized;
(4) vertically silica tube is placed, it is heated, make the raw materials melt in silica tube, in melting process, silica tube swings along its central shaft, cools under silica tube being placed in rapidly after melting the temperature of 10-20 DEG C, silica tube is broken after the liquid in silica tube solidifies completely, products obtained therefrom is magnesium-yittrium alloy, and in magnesium-yittrium alloy, yttrium content is 20wt% ~ 38wt%;
In step (2), the volume ratio of magnesium powder and yttrium powder is 1:1.
2. preparation method according to claim 1, is characterized in that: the angle that silica tube swings is up to 90 °.
3. preparation method according to claim 2, is characterized in that: the angle that silica tube swings is 60 ~ 90 °.
4. preparation method according to claim 1 and 2, is characterized in that: in step (2), and block density is 70% ~ 80%.
5. the preparation method according to any one of claim 1-3, is characterized in that: in step (4), after melting, silica tube is put into rapidly the salt solution that temperature is 10-20 DEG C, concentration is 15 ~ 25wt% and cools; In step (4), rise to 780 DEG C ~ 830 DEG C with the temperature rise rate of 2 ~ 8 DEG C/min and melting is carried out to raw material.
6. the preparation method according to any one of claim 1-3, is characterized in that: in silica tube, and magnesium grain is dispersed in around magnesium yttrium block; Vacuum tightness in silica tube is 0.1Pa ~ 1Pa.
7. the preparation method according to any one of claim 1-3, is characterized in that: gained magnesium-yttrium block adds in silica tube after drying at 100-120 DEG C again.
8. the preparation method according to any one of claim 1-3, is characterized in that: the quality purity of Mg powder and Y powder is all more than or equal to 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.
9. the preparation method according to any one of claim 1-3, 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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| CN100384777C (en) * | 2004-04-14 | 2008-04-30 | 中国科学院电工研究所 | Process for preparing magnesium diboride superconductor |
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