CN110340367A - The solid sintering preparation method of magnesium scandium alloy - Google Patents
The solid sintering preparation method of magnesium scandium alloy Download PDFInfo
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- CN110340367A CN110340367A CN201910713182.XA CN201910713182A CN110340367A CN 110340367 A CN110340367 A CN 110340367A CN 201910713182 A CN201910713182 A CN 201910713182A CN 110340367 A CN110340367 A CN 110340367A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
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Abstract
The present invention provides a kind of solid sintering preparation methods of magnesium scandium alloy.Method includes the following steps: S1, magnesium granules and scandium particle are mixed by way of stirring or grinding, magnesium scandium hybrid particles are obtained;Magnesium scandium hybrid particles are carried out under conditions of 200~400 DEG C of temperature, 200~600MPa of pressure hot pressing, form magnesium scandium mixture block by S2;Magnesium scandium mixture block is squeezed under conditions of 200~500 DEG C of temperature, extrusion ratio 5~30, obtains magnesium scandium alloy by S3.It is simple using this method process, and the advantage uniform with alloying component, scandium utilization rate is high.
Description
Technical field
The present invention relates to alloy manufacturing technology fields, are sintered preparation side in particular to a kind of solid of magnesium scandium alloy
Method.
Background technique
Magnesium scandium alloy due to excellent intensity, specific strength, plasticity, fatigue resistance, high temperature creep, high-termal conductivity and
Shape memory etc. can be widely applied to that rail traffic, automobile, aerospace, army's industry science be anti-and the fields such as communication electronics.
The preparation method of existing magnesium scandium alloy mainly has to the method for mixing, metallothermic processes and fused salt electrolysis process.It is to the method for mixing
In the Serum Magnesium that metal scandium is added directly into fusing under protective atmosphere, casts and be made after constant temperature stirring, but magnesium and scandium
Fusing point differ greatly so that method required temperature is high, constant temperature time is long to mixing, magnesium scandium scaling loss is serious, and the fusion of magnesium scandium is uneven,
Alloy structure component segregation is serious.Metallothermic processes is reducing agent using active metal magnesium to contain scadium compound as raw material, high
The lower scandium raw material of temperature is reduced to metal scandium in Serum Magnesium, and the metal scandium of generation is spread into Serum Magnesium, when in melt scandium it is dense
Degree is when reaching specified value, and casting obtains magnesium scandium alloy, but can generate toxic gas preparing the fused salt stage, and the casting yield of scandium compared with
Low, waste residue amount is big.Fused salt electrolysis process is will to contain scandium raw material to be added in specific molten-salt electrolysis plastidome, in the effect of electric field
Under, the scandium ion reduction in electrolyte forms metal scandium, and then forms magnesium scandium alloy, but required device is complicated, need to often replace
The conversion ratio of electrolytic cell, scandium is not high, and intermediate alloy preparation cost is high, has a large amount of solid waste fused salts to generate, causes to environment certain
Pollution.
Alloy is prepared using founding preparation process in patent CN102650010, first each component ingot in alloy exists
Mixed gas protected lower fusing, is then cast in mold and 750 DEG C keep the temperature 120 minutes, and last water cooling to room temperature is consolidated again
Molten (0.85Tm, 6h) and timeliness (0.2Tm, 2h, 80MPa) and it handles and the magnesium scandium alloy of obtained high creep resistance energy.However, due to
Magnesium, scandium chemical property are active, and the easily scaling loss in melting preparation process causes scandium utilization rate lower, higher cost, alloy melting
It is by the way of once all adding, alloying component tissue generates segregation unevenly, additionally needs subsequent solid solution and timeliness
Processing, complex process, high expensive.
Article " Mechanical properties of Mg-Sc binary alloys under compression "
In mention, Mg-Sc alloy is made using induction heating under vacuum in graphite crucible in commercial pure magnesium and scandium, and carries out to ingot casting equal
Processing (15h, 350 DEG C, Ar) is homogenized, the magnesium scandium alloy that intensity and toughness are improved is obtained.However, vacuum plant equipment is multiple
It is miscellaneous, prepare that sample is small not to be suitable for mass production application, and the content of scandium is lower, the excellent performance of scandium cannot fully demonstrate.
Complex chlorides first are made through chlorinating dissolution, filtering, evaporation, melting in scandium oxide in patent CN100546456 to melt
Salt recycles magnesium reduction process to prepare aluminium-magnesium-scandium master alloy.However, quoting strong acid in the technical process, subsequent technique needs
It removes again, increases process flow, final products are not pure magnesium scandium alloys, and it is 1.5%~3% (weight that scandium content is lower in alloy
Measure percentage), and it is not easy to control.
As it can be seen that there are complex procedures more in the method for preparing magnesium scandium alloy at present, alloying component is segregated uneven, scandium utilization rate
Low defect.
Summary of the invention
The main purpose of the present invention is to provide a kind of solid sintering preparation methods of magnesium scandium alloy, to solve the prior art
Middle complex procedures when preparing magnesium scandium alloy, the problem that alloying component segregation is uneven, scandium utilization rate is low.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of solid of magnesium scandium alloy is sintered system
Preparation Method comprising following steps: magnesium granules and scandium particle are mixed by way of stirring or grinding, obtain magnesium by S1
Scandium hybrid particles;Magnesium scandium hybrid particles are carried out hot pressing under conditions of 200~400 DEG C of temperature, 200~600MPa of pressure by S2,
Form magnesium scandium mixture block;S3, by magnesium scandium mixture block under conditions of 200~500 DEG C of temperature, extrusion ratio 5~30 into
Row squeezes, and obtains magnesium scandium alloy.
Further, in step S2, the hot pressing time of hot pressing is 5~180min.
Further, in step S2, by magnesium scandium hybrid particles in 300~400 DEG C of temperature, the item of 200~600MPa of pressure
120~180min of hot pressing is carried out under part, forms magnesium scandium mixture block.
Further, in step S3, the extrusion speed of extrusion process is 0.1~10mm/s.
Further, in step S3, by magnesium scandium mixture block in 200~500 DEG C of temperature, extrusion ratio 5~10, extruding speed
It is squeezed under conditions of 0.1~5mm/s of degree, obtains magnesium scandium alloy.
Further, in step S1, the partial size of magnesium granules is 50~300 mesh, purity >=99.0wt%;The partial size of scandium particle
For 50~300 mesh, purity >=99.5wt%.
Further, in magnesium scandium hybrid particles, the content of scandium element is 0.01~30.0wt%.
Further, in step S2, magnesium scandium hybrid particles is placed in sintered-carbide die and carry out hot pressing, and in heat
After pressing through journey, sintered-carbide die is cooled to room temperature, obtains magnesium scandium mixture block.
Further, in step S3, magnesium scandium mixture block is subjected to extrusion process in vertical extruder.
According to another aspect of the present invention, a kind of magnesium scandium alloy is additionally provided, is prepared by above-mentioned preparation method.
The present invention provides a kind of solid sintering preparation methods of magnesium scandium alloy comprising following steps: S1, by magnesium granules
It is mixed by way of stirring or grinding with scandium particle, obtains magnesium scandium hybrid particles;S2, by magnesium scandium hybrid particles in temperature
200~400 DEG C, hot pressing is carried out under conditions of 200~600MPa of pressure, form magnesium scandium mixture block;S3, by magnesium scandium mixture
Block is squeezed under conditions of 200~500 DEG C of temperature, extrusion ratio 5~30, obtains the magnesium scandium alloy.Using this method
Process is simple, and the advantage uniform with alloying component, scandium utilization rate is high.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the apparent photo of the magnesium scandium alloy material of 1 preparation according to embodiments of the present invention;
Fig. 2 shows the microstructures of the magnesium scandium alloy material of 1 preparation according to embodiments of the present invention to scan shape appearance figure;
Fig. 3 shows the microstructure scanning shape appearance figure of the magnesium scandium alloy material of 3 preparation according to embodiments of the present invention;And
Fig. 4 shows the apparent photo for the magnesium scandium alloy material that according to the present invention prepared by comparative example 1.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
As described in background technology part, in the prior art when preparing magnesium scandium alloy, there are complex procedures more, closes
The defects such as golden component segregation is uneven, scandium utilization rate is low.
To solve the above-mentioned problems, the present invention provides a kind of solid sintering preparation methods of magnesium scandium alloy comprising with
Lower step: S1 mixes magnesium granules and scandium particle by way of stirring or grinding, and obtains magnesium scandium hybrid particles;S2, will
Magnesium scandium hybrid particles carry out hot pressing under conditions of 200~400 DEG C of temperature, 200~600MPa of pressure, form magnesium scandium mixture block
Body;S3 squeezes magnesium scandium mixture block under conditions of 200~500 DEG C of temperature, extrusion ratio 5~30, obtains the conjunction of magnesium scandium
Gold.
Present invention employs a kind of modes of solid sintering to be prepared for magnesium scandium alloy, in above-mentioned preparation method, first using stirring
The mode mixed or ground mixes magnesium granules and scandium particle, this is just to prevent the component segregation of magnesium scandium in the finished alloy from beating
Basis has been descended, has been distributed each component in final magnesium scandium alloy more uniform.By magnesium scandium hybrid particles in specific temperature and
Hot pressing is carried out under pressure, which is less than the fusing point of magnesium scandium, and hot pressing is equivalent to solid state sintering process, and because of magnesium scandium
Eutectic temperature is also below magnesium scandium fusing point, after carrying out hot pressing under above-mentioned temperature and pressure, magnesium in the magnesium scandium mixture block of formation
Continuity between scandium is preferable, and interfacial effect is low.After by heat-press step, the present invention is further in specific temperature and extruding
Hot extrusion is carried out to magnesium scandium mixture block than under the conditions of, this, which is equivalent to, implements further solid state sintering, ultimately forms
The magnesium scandium alloy of ingredient even tissue.And because the temperature in hot pressing is lower than the fusing point of magnesium scandium magnesium scandium, avoiding problems magnesium scandiums
Melting scaling loss, so that magnesium and scandium is all had lower burn out rate, the utilization rate of the two is higher, and the scandium content of obtained alloy is more leaned on
Nearly design content.Meanwhile preparation method process provided by the invention is simple, is also suitble to industrialization large-scale application.
In order to further strengthen the effect of solid state sintering, in a preferred embodiment, in above-mentioned steps S2, hot pressing
The hot pressing time of process is 5~180min.It is highly preferred that in above-mentioned steps S2, by magnesium scandium hybrid particles in temperature 300~400
DEG C, 120~180min of hot pressing is carried out under conditions of 200~600MPa of pressure, form magnesium scandium mixture block.In above-mentioned technique item
Hot-pressing processing is carried out under part, the utilization rate of scandium is higher, and burn out rate is lower, and the continuity in magnesium scandium mixture block between magnesium scandium
More preferably, interfacial effect is lower.
In order to further strengthen the effect of solid state sintering, in a preferred embodiment, in above-mentioned steps S3, squeeze
The extrusion speed of process is 0.1~10mm/s.It is highly preferred that in above-mentioned steps S3, by magnesium scandium mixture block temperature 200~
500 DEG C, extrusion ratio 5~10, squeezed under conditions of 0.1~5mm/s of extrusion speed, obtain magnesium scandium alloy.In the technique item
Hot extrusion process is carried out under part, is conducive to the distribution for further improving magnesium scandium component in alloy, and amalgamation between the two is higher.
In a preferred embodiment, in above-mentioned steps S1, the partial sizes of magnesium granules is 50~300 mesh, purity >=
99.0wt%;The partial size of scandium particle is 50~300 mesh, purity >=99.5wt%.Using the magnesium granules of above-mentioned granularity and purity and
Scandium particle, two kinds of components of the magnesium scandium alloy of formation are more uniformly spread.
It is suitble to the range of the scandium content of production wider using the above-mentioned preparation method of the present invention, in a kind of preferred embodiment
In, in above-mentioned magnesium scandium hybrid particles, the content of scandium element is 0.01~30.0wt%.
In a preferred embodiment, in above-mentioned steps S2, magnesium scandium hybrid particles are placed in sintered-carbide die
Hot pressing is carried out, and after hot pressing, sintered-carbide die is cooled to room temperature, magnesium scandium mixture block is obtained.
It is highly preferred that magnesium scandium mixture block is carried out extrusion process in vertical extruder in above-mentioned steps S3.
According to another aspect of the present invention, a kind of magnesium scandium alloy is provided, is prepared by above-mentioned preparation method.As before
Described in text, because present invention employs by magnesium granules and scandium particle first mix dispersion, again first time solid state sintering (heat-press step), after
The technique of second of solid state sintering (hot extrusion process), magnesium scandium distributed components, scandium utilization rate are high in the magnesium scandium alloy.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
Embodiment 1
The solid state sintering of present embodiment prepares the technique of magnesium scandium alloy according to the following steps:
(1) weigh scandium powder 1.0g (having a size of 50 mesh, purity 99.5wt.%), the pure magnesium granules of 49.0g (having a size of 50 mesh,
Purity is 99.0wt.%), it is mixed with agitating mode, obtains magnesium scandium particle mixed-powder;
(2) mixed-powder for weighing appropriate step (1), mixed-powder is placed in sintered-carbide die, then mold is pre-
Heat sets pressure as 200MPa to 400 DEG C, and setting time 180min is then cooled to room temperature, and obtains magnesium scandium mixture block
Body;
(3) by the magnesium scandium mixture block in step (2) in vertical extruder with extrusion ratio be 10, squeeze temperature be
200 DEG C, the technological parameter of extrusion speed 5mm/s is squeezed, and obtains the magnesium scandium alloy material of the 2.0wt.% containing scandium, scandium it is paid
Rate is 99.4%.And the apparent photo of magnesium scandium alloy material is shown in that Fig. 1, microstructure scanning shape appearance figure are shown in Fig. 2.
Embodiment 2
The solid state sintering of present embodiment prepares the technique of magnesium scandium alloy according to the following steps
(1) it weighs scandium powder 0.01g (having a size of 200 mesh, purity 99.9wt.%), the pure magnesium granules of 99.99g (having a size of
300 mesh, purity 99.9wt.%), it is mixed using lapping mode, obtains magnesium scandium particle mixed-powder;
(2) mixed-powder for weighing appropriate step (1), mixed-powder is placed in sintered-carbide die, then mold is pre-
Heat sets pressure as 600MPa to 300 DEG C, and setting time 120min is then cooled to room temperature, and obtains magnesium scandium mixture block
Body;
(3) by the magnesium scandium mixture block in step (2) in vertical extruder with extrusion ratio be 5, squeeze temperature be 500
DEG C, the technological parameter of extrusion speed 0.1mm/s is squeezed, obtain the magnesium scandium alloy material of the 0.01wt.% containing scandium, scandium it is paid
Rate is 99.6%.
Embodiment 3
The solid state sintering of present embodiment prepares the technique of magnesium scandium alloy according to the following steps:
(1) scandium powder 2.0g (having a size of 100 mesh, purity 99.95wt.%) are weighed, the pure magnesium granules of 48.0g are (having a size of 200
Mesh, purity 99.99wt.%), it is mixed using lapping mode, obtains magnesium scandium particle mixed-powder;
(2) mixed-powder for weighing appropriate step (1), mixed-powder is placed in sintered-carbide die, then mold is pre-
Heat sets pressure as 300MPa to 200 DEG C, and setting time 30min is then cooled to room temperature, and obtains magnesium scandium mixture block;
(3) by the magnesium scandium mixture block in step (2) in vertical extruder with extrusion ratio be 30, squeeze temperature be
500 DEG C, the technological parameter of extrusion speed 10mm/s is squeezed, and obtains the magnesium scandium alloy material of the 4.0wt.% containing scandium, the reality of scandium
Yield is 99.2%.And the microstructure scanning shape appearance figure of magnesium scandium alloy material is shown in Fig. 3.
Embodiment 4
The solid state sintering of present embodiment prepares the technique of magnesium scandium alloy according to the following steps:
(1) it weighs scandium powder 15.0g (having a size of 100 mesh, purity 99.95wt.%), the pure magnesium granules of 35.0g (having a size of
100 mesh, purity 99.98wt.%), it is mixed using agitating mode, obtains magnesium scandium particle mixed-powder;
(2) mixed-powder for weighing appropriate step (1), mixed-powder is placed in sintered-carbide die, then mold is pre-
Heat sets pressure as 600MPa to 200 DEG C, and setting time 5min is then cooled to room temperature, and obtains magnesium scandium mixture block;
(3) by the magnesium scandium mixture block in step (2) in vertical extruder with extrusion ratio be 16, squeeze temperature be
350 DEG C, the technological parameter of extrusion speed 0.5mm/s is squeezed, and obtains the magnesium scandium alloy material of the 30wt.% containing scandium, the reality of scandium
Yield is 98.3%.
Embodiment 5
The solid state sintering of present embodiment prepares the technique of magnesium scandium alloy according to the following steps:
(1) weigh scandium powder 10g (having a size of 100 mesh, purity 99.98wt.%), the pure magnesium granules of 90g (having a size of 200 mesh,
Purity is 99.99wt.%), it is mixed using agitating mode, obtains magnesium scandium particle mixed-powder;
(2) mixed-powder for weighing appropriate step (1), mixed-powder is placed in sintered-carbide die, then mold is pre-
Heat sets pressure as 500MPa to 250 DEG C, and setting time 60min is then cooled to room temperature, and obtains magnesium scandium mixture block;
(3) by the magnesium scandium mixture block in step (2) in vertical extruder with extrusion ratio be 20, squeeze temperature be
350 DEG C, the technological parameter of extrusion speed 1.0mm/s is squeezed, and obtains the magnesium scandium alloy material of the 10wt.% containing scandium, the reality of scandium
Yield is 98.7%.
Comparative example 1
Preparation process difference from Example 1 is in the comparative example, and squeezing temperature is 150 DEG C.Its magnesium scandium alloy material
The apparent photo of material is shown in Fig. 4.
By comparison it will be evident that preparing magnesium scandium alloy using method provided by the invention, process is simple, alloying component
Uniformly, meanwhile, there is the high advantage of scandium utilization rate compared to other methods.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of solid sintering preparation method of magnesium scandium alloy, which is characterized in that the preparation method comprises the following steps:
S1 mixes magnesium granules and scandium particle by way of stirring or grinding, and obtains magnesium scandium hybrid particles;
The magnesium scandium hybrid particles are carried out hot pressing, shape under conditions of 200~400 DEG C of temperature, 200~600MPa of pressure by S2
At magnesium scandium mixture block;
The magnesium scandium mixture block is squeezed under conditions of 200~500 DEG C of temperature, extrusion ratio 5~30, is obtained by S3
The magnesium scandium alloy.
2. preparation method according to claim 1, which is characterized in that in the step S2, the hot pressing of the hot pressing
Time is 5~180min.
3. preparation method according to claim 2, which is characterized in that in the step S2, by the magnesium scandium hybrid particles
120~180min of hot pressing is carried out under conditions of 300~400 DEG C of temperature, 200~600MPa of pressure, forms the magnesium scandium mixing
Object block.
4. preparation method according to any one of claim 1 to 3, which is characterized in that in the step S3, the extruding
The extrusion speed of process is 0.1~10mm/s.
5. the preparation method according to claim 4, which is characterized in that in the step S3, by the magnesium scandium mixture block
Body is squeezed under conditions of 200~500 DEG C of temperature, extrusion ratio 5~10,0.1~5mm/s of extrusion speed, obtains the magnesium
Scandium alloy.
6. preparation method according to any one of claim 1 to 3, which is characterized in that in the step S1, the magnesium
The partial size of grain is 50~300 mesh, purity >=99.0wt%;The partial size of the scandium particle be 50~300 mesh, purity >=
99.5wt%.
7. preparation method according to claim 6, which is characterized in that in the magnesium scandium hybrid particles, the content of scandium element
For 0.01~30.0wt%.
8. preparation method according to any one of claim 1 to 3, which is characterized in that in the step S2, by the magnesium
Scandium hybrid particles, which are placed in sintered-carbide die, carries out the hot pressing, and after the hot pressing, will be described hard
Matter alloy mold is cooled to room temperature, and obtains the magnesium scandium mixture block.
9. preparation method according to any one of claim 1 to 3, which is characterized in that in the step S3, by the magnesium
Scandium mixture block carries out the extrusion process in vertical extruder.
10. a kind of magnesium scandium alloy, which is characterized in that the preparation method as described in any one of claims 1 to 9 is prepared.
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CN111250696A (en) * | 2020-04-05 | 2020-06-09 | 重庆大学 | Method for preparing magnesium rare earth alloy spectrum standard sample |
CN111250696B (en) * | 2020-04-05 | 2021-04-16 | 重庆大学 | Method for preparing magnesium rare earth alloy spectrum standard sample |
CN111455207A (en) * | 2020-04-08 | 2020-07-28 | 中国恩菲工程技术有限公司 | Method for preparing magnesium-scandium alloy by precursor process and magnesium-scandium alloy prepared by method |
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