CN109252142A - A kind of aluminium-scandium alloy target blankss and its preparation method and application - Google Patents
A kind of aluminium-scandium alloy target blankss and its preparation method and application Download PDFInfo
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- CN109252142A CN109252142A CN201811144477.1A CN201811144477A CN109252142A CN 109252142 A CN109252142 A CN 109252142A CN 201811144477 A CN201811144477 A CN 201811144477A CN 109252142 A CN109252142 A CN 109252142A
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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
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
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Abstract
The invention discloses a kind of aluminium-scandium alloy target blankss for belonging to aluminium-scandium alloy technical field and its preparation method and application.The present invention passes through aluminium-scandium alloy target blankss oxygen content < 100ppm prepared by cold crucible levitation melting combination variable frequency electromagnetic stirring, the sum of the mass percent of aluminium, scandium element > 99.95%, with high purity and oxygen content is low, is conducive to later period high quality and forms a film；Secondary-precipitated phase percentage by volume is 5~25% in aluminium-scandium alloy target blankss, average-size is 20~45 μm, shape is polygon and subsphaeroidal, microstructure is uniform, target blankss consistency is significantly improved, the formation that the internal flaws such as micro-crack in ingot casting and process of deformation can effectively be avoided, significantly improves target quality and yield rate.
Description
Technical field
The invention belongs to aluminium-scandium alloy technical field, in particular to a kind of aluminium-scandium alloy target blankss and preparation method thereof and answer
With.
Background technique
ScAlN piezoelectric film have praetersonic velocity of wave, high heat conductance, low dielectric loss, superior heat-stability, can with it is mutual
The advantages that mending metal-oxide semiconductor (MOS) (CMOS) process compatible, becomes and prepares high frequency, high power and highly integrated piezoelectric element
Ideal material.With the attention that the high speed development and various countries of science and technology study key area with critical material, aluminium-scandium alloy target
Critical material needed for base is prepared as ScAlN piezoelectric membrane, demand are growing.
Scandium content, the microstructure of aluminium-scandium alloy target blankss are an important factor for influencing the performance of ScAlN piezoelectric film.Gold
Belong to 1541 DEG C of scandium fusing point, chemical property is active, differs larger with 660 DEG C of fusing point of aluminium, common Medium frequency induction fusion casting preparation
Aluminium-scandium alloy ingot casting have that segregation is serious, and the mass percentage of scandium is only capable of reaching 0.05~2%, and secondary-precipitated phase is dendritic
Structure and coarseer, seriously affects the using effect of scandium-aluminum alloy target blankss.Patent CN201610677045.1 provides one kind
The preparation method of the aluminium-scandium alloy of high scandium content, the mass percentage of scandium can reach 55~70%, but vacuum powder sintering work
Skill has that oxygen content is high, consistency is low, influences the using effect of target.
Therefore, a kind of uniform raffinal scandium alloy target blankss of microstructure are researched and developed, for Micro Electro Mechanical System
(MEMS) etc. the development of devices sputtering target material is of great practical significance.
Summary of the invention
The purpose of the present invention is to provide a kind of aluminium-scandium alloy target blankss and its preparation method and application, and specific technical solution is such as
Under:
A kind of aluminium-scandium alloy target blankss, containing percentage by volume be 5~25%, 20~45 μm of average-size, shape are polygon
Shape and subsphaeroidal secondary-precipitated phase；In the secondary-precipitated phase, aggregate percentage by volume < 30%, subsphaeroidal secondary precipitation
Phase volume percentage is greater than 60%；Wherein secondary-precipitated phase is Al3Sc、Al2Sc、AlSc、AlSc2, one of Sc monomer phase or
The precipitated phase of multicomponent composition.
The sum of mass percent of aluminium, scandium element > 99.95% in the aluminium-scandium alloy target blankss, oxygen content < 100ppm,
Remaining is inevitable impurity.
The preparation methods of the aluminium-scandium alloy target blankss the following steps are included:
(1) in the target component ratio ingredient of the aluminium-scandium alloy target blankss, aluminium scandium raw material is placed in the water of suspension smelting furnace
In cold copper crucible, it is filled with argon gas, substep promotes monitor system, raw metal is completely melt；Use bifrequency induction power supply for
The suspension smelting furnace provides heat source.
Wherein, aluminium scandium raw material is fine aluminium and one of pure scandium, fine aluminium and aluminium-bearing master alloy, the aluminium-scandium alloy of fritting.
Preferably, it uses fine aluminium and aluminium-bearing master alloy for raw material, can reduce smelting temperature, shorten smelting time, subtract
Few metal scandium scaling loss, ingredient tend to be more uniform, controllable.
More preferably, it is preferred to use aluminium-bearing master alloy that fine aluminium and stoichiometric ratio are Al-87Sc is raw material, fusing point
Only 984 ± 5 DEG C, 557 ± 5 DEG C are differed with 1541 DEG C of fusing point of pure metal scandium, reduces alloying temperature.
Wherein, when aluminium scandium raw material is fine aluminium and pure scandium, fine aluminium and aluminium-bearing master alloy, water cooling earthenware is placed in using by fine aluminium
Crucible bottom, pure scandium or aluminium-bearing master alloy are placed in the mode on fine aluminium, the melting in the water jacketed copper crucible of suspension smelting furnace.
Wherein, the smelting temperature of aluminium scandium raw material be higher than 50~100 DEG C of alloying component liquidus point, vacuum degree be 0.08~
0.06MPa keeps the temperature 5~20min after being warming up to smelting temperature.
Wherein, substep promotes monitor system and is specially every graduated increasing 20kW, maintains heating 2min.
(2) reducing monitor system reduces melt temperature obtained by step (1), and opens electromagnetic agitation and melt is sufficiently stirred.
Wherein, in step (2) temperature-fall period, by melt temperature obtained by step (1) be reduced to alloying component liquidus point with
It is 0~80 DEG C lower, it is preferably decreased to alloying component liquidus point, rate of temperature fall is 5~10 DEG C/min.
During step (2) electromagnetic agitation, pass through the method for bifrequency induction power supply periodically output intermediate frequency and high frequency
Frequency conversion type electromagnetic agitation is carried out, the state for reaching turbulent flow inside metal bath is made；Wherein, when 6~15kHz of IF frequency, output
Between be 1~5S；Higher frequency 100-300kHz, output time are 5~20S；The electromagnetic agitation time is 5~15min.
The reinforcing agitating mode of variable frequency electromagnetic stirring in step (2), so that the secondary-precipitated phase of alloy is tiny, regular and equal
Even distribution, improves secondary-precipitated phase percentage by volume accounting, and secondary-precipitated phase appearance is from polygon to subsphaeroidal transformation；Nearly ball
Shape secondary-precipitated phase is conducive to improve target blankss consistency, effectively to avoid lacking inside micro-crack etc. in ingot casting and process of deformation
Sunken formation improves target quality and yield rate.
(3) melt obtained by step (2) is cast in mold, furnace cooling forms to arrive the aluminium-scandium alloy target
Base.
It is compared with the secondary-precipitated phase of dendritic morphology common in the art, in aluminium-scandium alloy target blankss obtained by the preparation method
Secondary-precipitated phase is the polygon and subsphaeroidal pattern of dispersion, and precipitated phase aggregate is few, microstructure is uniform, the purity of target blankss
High, hypoxic feature can also effectively avoid paradoxical discharge or spattering problem of the target blankss in sputtering process, after capable of guaranteeing
Phase high quality film forming.
The aluminium-scandium alloy target blankss are fixed on the target obtained on backboard, can be applied to Micro Electro Mechanical System (MEMS)
The preparation of equal devices.
The invention has the benefit that the present invention is prepared using cold crucible levitation melting combination variable frequency electromagnetic stirring
The uniform raffinal scandium alloy target blankss of microstructure, gained target blankss can sputter to form aluminium scandium film, may be used also as sputtering source
To obtain, a kind of piezoelectric response is high, the piezoelectric film with aluminium nitride film；It is compared with prior art processes, method letter
Single, properties of product are stablized, easy industrialized production.
Detailed description of the invention
Attached drawing 1 is that the secondary-precipitated phase of aluminium-scandium alloy target blankss in embodiment 3 is in the photo of nearly ball-type pattern；
Attached drawing 2 is that the secondary-precipitated phase of aluminium-scandium alloy target blankss in comparative example 1 is in the photo of dendritic morphology.
Specific embodiment
The present invention provides a kind of aluminium-scandium alloy target blankss and preparation method thereof, below with reference to embodiment and attached drawing to the present invention
It is described further.
Embodiment 1
Smelting equipment uses 10kg vacuum suspension furnace, and induction power supply is 8kHz intermediate frequency and the real-time dual output electricity of 200kHz high frequency
Source.
According to the composition proportion of aluminium-scandium alloy, it is (pure to weigh metal scandium 500g (purity 99.98%), metal aluminium ingot 5700g
Degree is 99.995%), metallic aluminium to be then placed in water jacketed copper crucible bottom, then metal scandium is placed in metal aluminum blocks；It closes
It is vacuumized after closed furnace lid, when vacuum degree reaches 0.5Pa, closes vacuum vacuum-pumping valve, be filled with high-purity argon gas to 0.07MPa, close
Close argon gas valve；Vacuum-pumping valve is beaten again, is evacuated to 0.1Pa, is continued to be filled with argon gas to 0.07MPa, is started to warm up, gradually rise
High power is to 1060 DEG C of smelting temperature, and after keeping the temperature 10min at such a temperature, reducing power makes 970 DEG C of molten metal temperature, setting
Power supply intermediate frequency exports the time as 5S, and the high frequency output time is 20S, and power decrease speed is 10kW/min, opens power supply and stirs mould
Then formula, duration 10min open rapidly tilt pouring, aluminium-scandium alloy liquid are cast in mold, ingot casting cools to the furnace
Room temperature, molding obtain aluminium-scandium alloy target blankss.
Embodiment 2
Smelting equipment uses 10kg vacuum suspension furnace, and induction power supply is 8kHz intermediate frequency and the real-time dual output electricity of 200kHz high frequency
Source.
According to the composition proportion of aluminium-scandium alloy, metal scandium 1500g (purity 99.98%), metal aluminium ingot 5000g are weighed
Then metallic aluminium is placed in water jacketed copper crucible bottom, then metal scandium is placed in metal aluminum blocks by (purity 99.995%)；
It is vacuumized after closing bell, when vacuum degree reaches 0.06Pa, closes vacuum vacuum-pumping valve, be filled with high-purity argon gas to 0.07MPa,
Close argon gas valve；Vacuum-pumping valve is beaten again, is evacuated to 0.2Pa, is continued to be filled with argon gas to 0.06MPa, is started to warm up, gradually
Increased wattage is to 1330 DEG C of smelting temperature, and after keeping the temperature 15min at such a temperature, reducing power makes 1220 DEG C of molten metal temperature,
The power supply intermediate frequency output time is set as 4S, the high frequency output time is 10S, and power decrease speed is 15kW/min, opens power supply and stirs
Mode is mixed, then duration 10min opens rapidly tilt pouring, aluminium-scandium alloy liquid is cast in mold, ingot casting is cold with furnace
But to room temperature, molding obtains aluminium-scandium alloy target blankss.
Embodiment 3
Smelting equipment uses 10kg vacuum suspension furnace, and induction power supply is 8kHz intermediate frequency and the real-time dual output electricity of 200kHz high frequency
Source.
According to the composition proportion of aluminium-scandium alloy, 545g containing bearing master alloy, the metal that stoichiometric ratio is Al-87Sc are weighed
Then metallic aluminium is placed in water jacketed copper crucible bottom, then scandium bearing master alloy is put by aluminium ingot 5650g (purity 99.995%)
It is placed in metal aluminum blocks；It is vacuumized after closing bell, when vacuum degree reaches 0.5Pa, closes vacuum vacuum-pumping valve, be filled with high-purity
Argon gas closes argon gas valve to 0.07MPa；Vacuum-pumping valve is beaten again, is evacuated to 0.1Pa, continues to be filled with argon gas extremely
0.07MPa is started to warm up, and is gradually risen power to 1060 DEG C of smelting temperature, after keeping the temperature 20min at such a temperature, is reduced power
Make 970 DEG C of molten metal temperature, sets the power supply intermediate frequency output time as 2S, the high frequency output time is 5S, and power decrease speed is
20kW/min, opens power supply stirring mode, then duration 8min opens rapidly tilt pouring, aluminium-scandium alloy liquid is cast
Into mold, ingot casting cools to room temperature with the furnace, and molding obtains aluminium-scandium alloy target blankss.
Comparative example 1
Smelting equipment uses 1kg vacuum suspension furnace.
According to the composition proportion of aluminium-scandium alloy, metal scandium 29.0g (purity 99.98%), metal aluminium ingot 330g (purity are weighed
99.995%) metallic aluminium then, is placed in water jacketed copper crucible bottom, then metal scandium is placed in metal aluminum blocks；Close furnace
It is vacuumized after lid, when vacuum degree reaches 2Pa, closes vacuum vacuum-pumping valve, be filled with high-purity argon gas to 0.07MPa, close argon gas
Valve；Vacuum-pumping valve is beaten again, is evacuated to 2Pa, is continued to be filled with argon gas to 0.07MPa, is started to warm up, gradually rise power extremely
It 1100 DEG C of smelting temperature, after keeping the temperature 10min at such a temperature, casts；Aluminium-scandium alloy liquid is cast in mold, ingot casting with
Furnace is cooled to room temperature, and molding obtains aluminium-scandium alloy target blankss.
Measure oxygen content, secondary-precipitated phase and the impurity content of embodiment 1-3, aluminium-scandium alloy target blankss prepared by comparative example 1:
Oxygen content is measured using noble gas pulsed infrared thermal conductivity method；Using Metallography method determination (GB6394-86) embodiment 3, comparative example 1 two times
Content, size and the exterior appearance of precipitated phase；Using the content of GD-MS or ICP-MS analysing impurity, aluminium scandium is calculated by minusing
The purity of alloy target blankss；Testing result is as shown in table 1, Fig. 1, Fig. 2:
Table 1
Include the modes such as welding, occlusion using common technology means, aluminium-scandium alloy target blankss prepared by embodiment 1-3 are fixed
In obtaining aluminium-scandium alloy target on backboard, dorsulum is used to provide support for target blankss, and material is the material for meeting design requirement,
Such as copper backboard, copper alloy backing plate, gained target can apply to the preparation of the devices such as Micro Electro Mechanical System (MEMS).
Claims (10)
1. a kind of aluminium-scandium alloy target blankss, which is characterized in that the percentage by volume of secondary-precipitated phase is 5 in the aluminium-scandium alloy target blankss
~25%, average-size is 20~45 μm, shape is polygon and subsphaeroidal；In the secondary-precipitated phase, aggregate volume hundred
Score < 30%, subsphaeroidal percentage by volume are greater than 60%；
The oxygen content < 100ppm of the aluminium-scandium alloy target blankss, the sum of the mass percent > 99.95% of aluminium, scandium element.
2. aluminium-scandium alloy target blankss according to claim 1, which is characterized in that the secondary-precipitated phase is Al3Sc、Al2Sc、
AlSc、AlSc2, one of Sc or a variety of.
3. the preparation method of aluminium-scandium alloy target blankss as claimed in claim 1 or 2, which is characterized in that the preparation method includes following
Step:
(1) the suspension smelting furnace melting aluminium scandium raw material containing water jacketed copper crucible is utilized, until being completely melt；
(2) melt temperature obtained by step (1) is reduced, and carries out electromagnetic agitation；
(3) melt obtained by step (2) is cast, is cooled and shaped to get the aluminium-scandium alloy target blankss.
4. preparation method according to claim 3, which is characterized in that aluminium scandium raw material is fine aluminium and pure in the step (1)
One of scandium, fine aluminium and aluminium-bearing master alloy, the aluminium-scandium alloy of fritting.
5. the preparation method according to claim 4, which is characterized in that the aluminium scandium raw material be fine aluminium and pure scandium, fine aluminium and
Aluminium-bearing master alloy, is placed in cold-crucible bottom, pure scandium or aluminium-bearing master alloy for fine aluminium and is placed on fine aluminium and carry out melting.
6. preparation method according to claim 3, which is characterized in that step (1) melting carries out under argon gas, vacuum
Degree be 0.08~0.06MPa, smelting temperature be higher than 50~100 DEG C of alloying component liquidus point, under smelting temperature keep the temperature 5~
20min。
7. preparation method according to claim 6, which is characterized in that promote monitor system by substep and reach the melting
Temperature, specifically: every graduated increasing 20kW, maintain heating 2min.
8. preparation method according to claim 3, which is characterized in that in the step (2), by melt obtained by step (1)
Temperature is reduced to 0~80 DEG C of alloying component liquidus point or less, and rate of temperature fall is 5~10 DEG C/min, and the electromagnetic agitation time is 5~
15min。
9. preparation method according to claim 8, which is characterized in that the electromagnetic agitation by periodically export intermediate frequency and
The mode of high frequency carries out, and wherein IF frequency is 6~15kHz, and the output time is 1~5S；Higher frequency is 100-300kHz, defeated
The time is 5~20S out.
10. the preparation that aluminium-scandium alloy target blankss as claimed in claim 1 or 2 can apply to Micro Electro Mechanical System device.
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| CN110423921A (en) * | 2019-09-12 | 2019-11-08 | 中国恩菲工程技术有限公司 | A kind of ScAl3/ Al base composite inoculant, preparation method and application |
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| CN111455223A (en) * | 2019-08-08 | 2020-07-28 | 湖南稀土金属材料研究院 | Aluminum-scandium alloy target material and preparation method thereof |
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