CN106086567B - A kind of high scandium content aluminium-scandium alloy and preparation method thereof - Google Patents
A kind of high scandium content aluminium-scandium alloy and preparation method thereof Download PDFInfo
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- CN106086567B CN106086567B CN201610677045.1A CN201610677045A CN106086567B CN 106086567 B CN106086567 B CN 106086567B CN 201610677045 A CN201610677045 A CN 201610677045A CN 106086567 B CN106086567 B CN 106086567B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The present invention provides a kind of high scandium content aluminium-scandium alloy and preparation method thereof, belongs to high performance aluminium materials preparing technical field.In the high scandium content aluminium-scandium alloy, the weight percentage of scandium element is 55%~70%, remaining is aluminium element.Its preparation method includes：1) powder is sieved：Aluminium powder and scandium powder are crossed to the sieve of different meshes respectively, screen out the raw material of required granularity；2) dispensing：A certain amount of aluminium powder and scandium powder is weighed respectively, and aluminium powder, scandium powder are mixed according to certain mass ratio；3) grind：Aluminium scandium mixed powder is put into ball mill and is fully ground, is uniformly mixed it；4) sinter：Uniform aluminium scandium mixed powder will be ground and load mould, after carrying out precompressed using hydraulic press, shove charge simultaneously sets sintering procedure and is sintered and prepare aluminium-scandium alloy.The aluminium-scandium alloy prepared by the present invention has high consistency, scandium content height, the good characteristic of the good and follow-up machinability of homogeneity of ingredients, can provide reliable raw material with sputtering target material for special dimension.
Description
Technical field
The present invention relates to a kind of high scandium content aluminium-scandium alloy and preparation method thereof, which is mainly used for special dimension sputtering
Target, belongs to high performance aluminium materials preparing technical field.
Background technology
Certain scandium is added in aluminium, crystal grain thinning can be played, recrystallization temperature is improved, improve corrosion resistance, improve intensity
Acted on plasticity etc., therefore aluminium-scandium alloy has the good comprehensive performance of high intensity, corrosion resistance, high temperature resistant and solderability, is navigating
The field such as the hard-core technology such as empty space flight, nuclear energy engineering field and communications and transportation, household electrical appliance has a wide range of applications.With section
The high speed development of skill, and the attention that various countries study key area with critical material, to high scandium content aluminium-scandium alloy target
Demand also increasingly increases.
Both the fusing point of metal scandium is up to 1541 DEG C, and chemical property is active, differs larger with the fusing point of aluminium, when directly fusing
It is not easy to be uniformly mixed, the aluminium scadium compound coarse grains of formation, segregation is serious.When therefore preparing aluminium-scandium alloy, scandium must be in
Between alloy form add.Prepare before aluminium-scandium alloy, it is necessary to first pass through to the method for mixing, fused salt electrolysis process, metal thermit reduction
The methods of prepare contain bearing master alloy.And existing process prepare aluminium-scandium alloy in scandium content in the range of 0.05%~2.0%,
Aluminium-scandium alloy of the scandium content more than 10% yet there are no report.
Therefore, a kind of method for simply, quickly preparing high scandium content aluminium-scandium alloy is researched and developed, for key area
Be of great practical significance with the development of sputtering target material.
The content of the invention
It is an object of the present invention to provide a kind of high scandium content aluminium-scandium alloy.
The purpose of foregoing invention of the present invention, reaches by the following technical programs：
A kind of high scandium content aluminium-scandium alloy, it is characterised in that：The mass percentage of scandium element is 55%~70%, remaining
For aluminium element.
Preferably, the thickness of the alloy is 5~20mm, consistency >=99%.
Another object of the present invention provides a kind of method for simply, quickly preparing high scandium content aluminium-scandium alloy.
The purpose of foregoing invention of the present invention, reaches by the following technical programs：
A kind of high scandium content aluminium-scandium alloy, its preparation process are as follows：
1) aluminium powder and scandium powder are crossed to the sieve of different meshes respectively, screen out the raw material of required granularity；
2) weight of the required raw material aluminium of every stove sintering, scandium is calculated by the component content of aluminium-scandium alloy, is weighed respectively；
3) aluminium powder and scandium powder are mixed and are put into planetary ball mill, make Mechanical Alloying；
4) ground aluminium scandium mixed-powder is loaded into mould, precompressed, loads sintering furnace by mould, vacuumize, applying argon gas
Prepurging, then vacuumize, then, setting heating and pressurization protocols, applying argon gas, come out of the stove, and obtain aluminium-scandium alloy.
Preferably, the aluminium powder screened out described in the step 1) is 200 mesh, and scandium powder is 50~100 mesh.
Preferably, purity >=99.99wt% of aluminium powder described in the step 1)；The purity of the scandium powder >=
99.9wt%.
Preferably, the amount of scandium powder described in the step 2) is 55~70 weight %.
Preferably, the ball milling speed of planetary ball mill described in the step 3) is 200~800r/min, and rotating replaces
Be ground 2~5 it is small when.
Preferably, mould described in the step 4) is ceramic mold, graphite jig or sintered-carbide die.
Preferably, precompressed described in the step 4) is carried out using hydraulic press, and the pressure of the hydraulic press is 0~20MPa.
Preferably, the pressure vacuumized again described in the step 4) is 1 × 10-1~1 × 10-3MPa。
Preferably, setting heating described in the step 4) and pressurization protocols：Heating rate is set as 100 DEG C/min, is protected
The warm time is：10~30min, pressure are 45~70MPa.
Preferably, after obtaining the aluminium-scandium alloy in the step 4), the graphite paper of alloy surface is removed using sand-blasting machine,
Then grinding process sample, carries out the dependence tests such as consistency.
The present invention utilizes powder sintering, and the granularity, sintering process parameter by adjusting raw material reach guarantee alloying component
Uniformity, the purpose for improving alloy consistency.The thickness of aluminium-scandium alloy：5~20mm, consistency >=99%, the quality of scandium element
Percentage composition is 55%~70%, remaining is aluminium element.
Main advantages of the present invention：This method is easy to operate, the utilization rate of expensive metal scandium is high, be conducive to industrialization should
With.The aluminium-scandium alloy prepared by this method has consistency high (>=99%), scandium content high (55%~70%), homogeneity of ingredients
The good characteristic of good and follow-up machinability, meets the needs of special dimension sputtering target material.
Below by embodiment, the present invention will be further described, but is not meant to the scope of the present invention
Limitation.
Embodiment
Embodiment 1
By the aluminium powder of purity 99.99wt%, the scandium powder of purity 99.9wt% crosses the sieve of different meshes respectively, screens out
The scandium powder of the aluminium powder of 200 mesh and 50~100 mesh；The scandium powder of the aluminium powder of 200 mesh and 50~100 mesh is 45 by mass percentage:55
Ratio mixing.Put the powder into rotating in planetary ball mill and alternately grind 5h, rotational speed of ball-mill 300r/min.Then
Ground powder is loaded to the sintered-carbide die of Φ 60, utilizes hydraulic press precompressed under the pressure of 20MPa., will after precompressed
Mould loads sintering furnace.Vacuumize, applying argon gas prepurging, then be evacuated to 1 × 10-3MPa, sets heating rate as 100 DEG C/min,
Soaking time is 30min, and sintering pressure 65MPa, is sintered.Program end of run, applying argon gas, come out of the stove, and obtain the present invention
Aluminium-scandium alloy, be surface-treated, the graphite paper of alloy surface removed using sand-blasting machine, then grinding process sample, carries out
The dependence tests such as consistency.
Using the density of Archimedes's drainage test sample, and calculate the consistency of sample.Using ICP-AES (wait from
Sub- emission spectrometry), the performance of scanning electron microscope analysis sample.The thickness of prepared aluminium-scandium alloy is as stated above
10mm, consistency 99.20%, scandium content are 55wt%.
Embodiment 2
By the aluminium powder of purity 99.999%, the scandium powder of purity 99.99% crosses the sieve of different meshes respectively, screens out 200
The scandium powder of purpose aluminium powder and 50~100 mesh；The scandium powder of the aluminium powder of 200 mesh and 50~100 mesh is 40 by mass percentage:60 ratio
Example mixing.Put the powder into rotating in planetary ball mill and alternately grind 5h, rotational speed of ball-mill 300r/min.Then will grind
The powder of milled loads 40 sintered-carbide dies of Φ, utilizes hydraulic press precompressed under the pressure of 15MPa.After precompressed, mould is filled
Enter sintering furnace.Vacuumize, applying argon gas prepurging, then be evacuated to 1 × 10-3MPa, sets heating rate as 100 DEG C/min, during insulation
Between be 20min, pressure 55MPa, is sintered.Program end of run, applying argon gas, come out of the stove, and obtain the aluminium-scandium alloy of the present invention,
It is surface-treated, the graphite paper of alloy surface is removed using sand-blasting machine, then grinding process sample, carries out the correlations such as consistency
Test.
Using the density of Archimedes's drainage test sample, and calculate the consistency of sample.Using ICP-AES (wait from
Sub- emission spectrometry), the performance of scanning electron microscope analysis sample.The thickness of prepared aluminium-scandium alloy is as stated above
15mm, consistency 99.32%, scandium content are 60wt%.
Embodiment 3
By the aluminium powder of purity 99.99%, the scandium powder of purity 99.9% crosses the sieve of different meshes respectively, screens out 200 mesh
Aluminium powder and 50~100 mesh scandium powder；The scandium powder of the aluminium powder of 200 mesh and 50~100 mesh is 35 by mass percentage:65 ratio
Mixing.Put the powder into and 3h is ground in planetary ball mill, rotational speed of ball-mill 200r/min.Then ground powder is filled
Enter the graphite jig of Φ 30, utilize hydraulic press precompressed under the pressure of 10MPa.After precompressed, mould is loaded into sintering furnace.Take out true
Sky, applying argon gas prepurging, then it is evacuated to 1 × 10-2MPa, sets heating rate as 100 DEG C/min, soaking time 10min, pressure
Power is 45MPa, is sintered.Program end of run, applying argon gas, come out of the stove, and obtain the aluminium-scandium alloy of the present invention, carry out at surface
Reason, the graphite paper of alloy surface is removed using sand-blasting machine, then grinding process sample, carries out the dependence tests such as consistency.
Using the density of Archimedes's drainage test sample, and calculate the consistency of sample.Using ICP-AES (wait from
Sub- emission spectrometry), the performance of scanning electron microscope analysis sample.The thickness of prepared aluminium-scandium alloy is as stated above
10mm, consistency 99.69%, scandium content are 65wt%.
Embodiment 4
By the aluminium powder of purity 99.99%, the scandium powder of purity 99.9% crosses the sieve of different meshes respectively, screens out 200 mesh
Aluminium powder and 50~100 mesh scandium powder；The scandium powder of the aluminium powder of 200 mesh and 50~100 mesh is 30 by mass percentage:70 ratio
Mixing.Put the powder into and 2h is ground in planetary ball mill, rotational speed of ball-mill 200r/min.Then ground powder is filled
Enter the graphite jig of Φ 10, utilize hydraulic press precompressed under the pressure of 5MPa.After precompressed, mould is loaded into sintering furnace.Vacuumize,
Applying argon gas prepurging, then it is evacuated to 1 × 10-2MPa, sets heating rate as 100 DEG C/min, soaking time 10min, and pressure is
40MPa, is sintered.Program end of run, applying argon gas, come out of the stove, and obtain the aluminium-scandium alloy of the present invention, are surface-treated, profit
The graphite paper of alloy surface is removed with sand-blasting machine, then grinding process sample, carry out the dependence tests such as consistency.
Using the density of Archimedes's drainage test sample, and calculate the consistency of sample.Using ICP-AES (wait from
Sub- emission spectrometry), the performance of scanning electron microscope analysis sample.The thickness of prepared aluminium-scandium alloy is as stated above
10mm, consistency 99.62%, scandium content are 70wt%.
Aluminium-scandium alloy prepared by the present invention has consistency height, scandium content is high, homogeneity of ingredients is good and follow-up machinability
Good characteristic.Scandium content reaches more than 50% in alloy, alloy consistency >=99%.Can be that special dimension is carried with sputtering target material
For reliable raw material.
Only enumerate the partial content of the high scandium content aluminium-scandium alloy of the present invention in above-described embodiment, specific sintering pressure,
The parameter such as ball milling situation and soaking time, can be adjusted according to the thickness of mould size and required sample.Therefore more than
The technical solution that is included of explanation should be regarded as protection domain that is illustrative, and being not used to limitation the present patent application patent.
Claims (7)
- A kind of 1. high scandium content aluminium-scandium alloy, it is characterised in that：The weight percentage of scandium element is 55%~70%, remaining is Aluminium element, is prepared using following steps：1) aluminium powder and scandium powder are crossed to the sieve of different meshes respectively, screen out the original of required granularity Material, the aluminium powder screened out is 200 mesh, and scandium powder is 50~100 mesh；2) calculate every stove by the component content of aluminium-scandium alloy and sinter institute The raw material aluminium of need, the weight of scandium, weigh respectively；The weight percentage of scandium powder is 55%~70%, remaining is aluminium powder；3) by aluminium Powder and the mixing of scandium powder are put into planetary ball mill, make Mechanical Alloying；4) ground aluminium scandium mixed-powder is loaded into mould Tool, precompressed, loads sintering furnace by mould, vacuumizes, applying argon gas prepurging, then vacuumizes, then, setting heating and pressurization protocols, Heating rate is 100 DEG C/min, and soaking time is 10~30min, and pressure is 45~70MPa；Applying argon gas, come out of the stove, and obtain aluminium scandium Alloy.
- 2. high scandium content aluminium-scandium alloy according to claim 1, it is characterised in that：Consistency >=99% of the alloy； The thickness of the alloy is 5~20mm.
- 3. a kind of preparation method of high scandium content aluminium-scandium alloy, includes the following steps：1) aluminium powder and scandium powder are crossed to the sieve of different meshes respectively, screen out the raw material of required granularity, the aluminium powder screened out is 200 Mesh, scandium powder are 50~100 mesh；2) weight of the required raw material aluminium of every stove sintering, scandium is calculated by the component content of aluminium-scandium alloy, is weighed respectively；Scandium powder Weight percentage is 55%~70%, remaining is aluminium powder；3) aluminium powder and scandium powder are mixed and are put into planetary ball mill, make Mechanical Alloying；4) ground aluminium scandium mixed-powder being loaded into mould, precompressed, loads sintering furnace by mould, vacuumizes, applying argon gas prepurging, Vacuumize again, then, setting heating and pressurization protocols, heating rate are 100 DEG C/min, and soaking time is 10~30min, pressure For 45~70MPa；Applying argon gas, come out of the stove, and obtain aluminium-scandium alloy.
- 4. the preparation method of high scandium content aluminium-scandium alloy according to claim 3, it is characterised in that：The purity of the aluminium powder >=99.99%；Purity >=99.9% of the scandium powder.
- 5. the preparation method of high scandium content aluminium-scandium alloy according to claim 3, it is characterised in that：Institute in the step 3) The ball milling speed for stating planetary ball mill is 200~800r/min, rotating alternately grind 2~5 it is small when.
- 6. the preparation method of high scandium content aluminium-scandium alloy according to claim 3, it is characterised in that：Institute in the step 4) It is ceramic mold, graphite jig or sintered-carbide die to state mould.
- 7. the preparation method of high scandium content aluminium-scandium alloy according to claim 3, it is characterised in that：Institute in the step 4) It is hydraulic press to state prepressing means, and the pressure of the hydraulic press is 0~20MPa；The pressure vacuumized again is 1 × 10-1~1 × 10-3MPa。
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| CN108441827A (en) * | 2018-04-17 | 2018-08-24 | 长沙迅洋新材料科技有限公司 | Aluminium-scandium alloy target preparation method |
| CN110438458A (en) * | 2018-05-04 | 2019-11-12 | 何午琳 | A kind of high scandium content aluminium-scandium alloy sputtering target material and preparation method thereof |
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| CN111455327B (en) * | 2019-08-08 | 2022-04-12 | 湖南稀土金属材料研究院 | High-scandium-content aluminum-scandium alloy target material and preparation method thereof |
| CN110470140A (en) * | 2019-08-30 | 2019-11-19 | 王一浩 | A kind of aluminium-scandium alloy smelting waste separation scandium oxide recovery furnace |
| CN110714142A (en) * | 2019-11-06 | 2020-01-21 | 长沙迅洋新材料科技有限公司 | Al-Sc-X multi-element alloy target and preparation method thereof |
| CN111560585B (en) * | 2020-04-28 | 2022-07-01 | 先导薄膜材料（广东）有限公司 | Preparation method of aluminum scandium target material |
| CN113584443B (en) * | 2021-06-30 | 2023-03-21 | 武汉大学 | AlN/AlScN nano composite piezoelectric coating for high-temperature-resistant fastener and preparation method thereof |
| CN115537746B (en) * | 2022-10-25 | 2024-04-19 | 洛阳丰联科绑定技术有限公司 | Aluminum scandium alloy target material and preparation method and application thereof |
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