CN111647858B - Preparation method of aluminum-scandium alloy target material - Google Patents
Preparation method of aluminum-scandium alloy target material Download PDFInfo
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- CN111647858B CN111647858B CN202010492396.1A CN202010492396A CN111647858B CN 111647858 B CN111647858 B CN 111647858B CN 202010492396 A CN202010492396 A CN 202010492396A CN 111647858 B CN111647858 B CN 111647858B
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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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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
Abstract
The invention discloses a preparation method of an aluminum-scandium alloy target material, which comprises the following steps: carrying out suspension smelting on an aluminum raw material and a scandium raw material through a cold crucible to obtain an aluminum-scandium alloy melt; casting the aluminum-scandium alloy melt onto a mould for cooling and forming to obtain an aluminum-scandium alloy ingot; placing the aluminum-scandium alloy cast ingot in a vacuum crucible furnace, and heating to melt the cast ingot into aluminum-scandium alloy liquid; atomizing the aluminum-scandium alloy liquid to obtain aluminum-scandium alloy powder; sintering the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy target blank; and machining the aluminum-scandium alloy target blank to obtain the aluminum-scandium alloy target. According to the preparation method of the aluminum-scandium alloy target, provided by the invention, the aluminum raw material is added into the scandium raw material in batches for smelting according to the characteristic that the metal melting points of aluminum and scandium are greatly different, so that the alloy target can be smelted to be completely alloyed, and the aluminum-scandium alloy powder with high product purity is prepared by adopting a melting and atomizing mode, so that the technical problem that the alloy phase splitting is caused when the aluminum-scandium alloy target is prepared in the prior art is solved.
Description
Technical Field
The invention relates to the technical field of high-performance aluminum-scandium alloy targets, in particular to a preparation method of an aluminum-scandium alloy target.
Background
Scandium has good alloying effect on alloy target material, and only a few thousandths of scandium is added into aluminum to generate Al which is dispersed and distributed 3 The Sc phase greatly refines the structure of the aluminum alloy, thereby improving the strength of the aluminum alloy, and the aluminum-scandium alloy target material has good performanceThe aluminum-scandium alloy has the advantages of corrosion resistance, excellent radiation resistance, lower resistivity, effective reduction of short circuit, better thermal stability, less protrusions before and after thin film heat treatment, no drastic change of comprehensive performance along with the change of heat treatment temperature and the like, can meet the requirements of coating and using of substrate electrode layers and large-scale integrated circuit wiring materials, and needs to be sputtered to form the aluminum-scandium alloy in various occasions, for example, in the preparation process of a micro-electromechanical system (MEMS) integrating a micro-sensor, an actuator, a signal processing and control circuit, an interface circuit and a communication and power supply.
The aluminum-scandium alloy target material is prepared by two methods, one method is prepared by a process of direct casting molding and then hot processing, and the other method is prepared by a powder metallurgy process. Although the aluminum-scandium alloy target material prepared by the process of direct casting molding and hot working has the advantages of easy molding, high purity, good component uniformity, low gas content and the like, researches show that when the scandium (Sc) content is more than 25at%, a simple substance aluminum phase is almost not present, so that the brittleness of the alloy is increased, and therefore the process of direct casting molding and hot working is only limited to the preparation of AlSc target materials with the Sc content below 25at% and the small-size scandium content higher than 25 at%. For casting of target blanks with higher Sc content or larger size, Al is a large amount of brittle particles in the matrix 3 Sc and Al 2 Sc, which easily causes cracking of the target blank during cooling or processing, can only be prepared by a powder metallurgy process.
In the prior art, a method for preparing an aluminum-scandium alloy target by a powder metallurgy process is disclosed, aluminum and scandium are directly smelted, smelting is difficult to reach complete alloying, and aluminum-scandium alloy powder with high product purity is difficult to prepare.
The existing preparation technology of the aluminum-scandium alloy target material has certain technical defects, and the technical problem is solved by combining the advantages of the technology in order to obtain the aluminum-scandium alloy target material which has the advantages of simple technology, short production period, low production cost, high product purity and low impurity content and meets the requirements of customers.
Aiming at the defects of the prior art, the invention provides a preparation method of an aluminum-scandium alloy target.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an aluminum scandium alloy target.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a preparation method of an aluminum-scandium alloy target, which comprises the following steps: smelting, namely performing suspension smelting on an aluminum raw material and a scandium raw material through a cold crucible to obtain an aluminum-scandium alloy melt; casting, namely casting the aluminum-scandium alloy melt onto a mould for cooling and forming to obtain an aluminum-scandium alloy cast ingot; melting, namely placing the aluminum-scandium alloy cast ingot in a vacuum crucible furnace, and heating to melt the cast ingot into aluminum-scandium alloy liquid; atomizing, namely atomizing the aluminum-scandium alloy liquid to obtain aluminum-scandium alloy powder; sintering, namely sintering the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy target blank; and machining, namely machining the aluminum-scandium alloy target blank to obtain the aluminum-scandium alloy target.
As a further improvement of the invention, the step melting is to perform suspension melting on an aluminum raw material and a scandium raw material through a cold crucible to obtain an aluminum-scandium alloy melt, which specifically comprises the following steps: the method comprises the steps of taking a scandium raw material and an aluminum raw material as reaction raw materials, firstly, suspending the scandium raw material through a cold crucible for smelting to obtain a scandium melt, and then adding the aluminum raw material into the scandium melt in batches for smelting to obtain an aluminum-scandium alloy melt.
As a further improvement of the invention, the step of placing the aluminum-scandium alloy ingot into a vacuum crucible furnace, and heating to melt the ingot into aluminum-scandium alloy liquid specifically comprises the following steps: and (3) placing the aluminum-scandium alloy ingot in a vacuum crucible, heating the ingot in the crucible to 1450-1650 ℃, wherein the heating duration is 25-35 min, melting the ingot in the crucible into aluminum-scandium alloy liquid, and then preserving heat for 5-20 min.
As a further improvement of the present invention, the step of atomizing the aluminum-scandium alloy liquid to obtain aluminum-scandium alloy powder specifically includes: and (3) enabling the aluminum scandium alloy liquid to flow out through an atomizing nozzle to meet gas flowing at a high speed, atomizing into fine droplets, and solidifying the droplets into aluminum scandium alloy powder in a closed atomizing chamber.
As a further improvement of the present invention, the step of sintering the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy target blank specifically includes: and (2) placing the aluminum-scandium alloy powder in a graphite mold, placing the graphite mold in a hot-pressing sintering furnace, raising the temperature and the pressure to 950-1150 ℃, keeping the pressure at 20-40 Mpa, then carrying out constant temperature and constant pressure for 100-240 min, and removing the pressure after the constant temperature and constant pressure are finished so as to cool the aluminum-scandium alloy powder to obtain the aluminum-scandium alloy powder target blank.
As a further improvement of the invention, the heating rate is 10-20 ℃/min.
As a further improvement of the invention, the boosting rate is 0.5-2 t/min.
As a further improvement of the invention, the casting time is 5-10S.
As a further improvement of the invention, the pressure of the gas flow is 2-3 MPa.
As a further improvement of the invention, the vacuum crucible furnace is one of an alumina vacuum crucible furnace, a zirconia vacuum crucible furnace or a magnesia vacuum crucible furnace.
According to the preparation method of the aluminum-scandium alloy target, provided by the invention, the aluminum raw material is added into the scandium raw material in batches for smelting according to the characteristic that the metal melting points of aluminum and scandium are greatly different, so that the alloy target can be smelted to be completely alloyed, and the aluminum-scandium alloy powder with high product purity is prepared by adopting a melting and atomizing mode, so that the technical problem that the alloy phase splitting is caused when the aluminum-scandium alloy target is prepared in the prior art is solved.
Drawings
Fig. 1 is an SEM image of the aluminum scandium alloy powder prepared in example 1 of the present invention.
Fig. 2 is a metallographic image of the surface of the aluminum-scandium alloy target material prepared in embodiment 1 before corrosion.
Fig. 3 is a metallographic image of the surface of the aluminum-scandium alloy target material prepared in example 1 after being corroded.
Detailed Description
The technical solutions will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of an aluminum-scandium alloy target, which comprises the following steps:
and smelting, namely performing suspension smelting on the aluminum raw material and the scandium raw material through a cold crucible to obtain an aluminum-scandium alloy melt.
Using scandium raw materials and aluminum raw materials as reaction raw materials, wherein the scandium raw materials are granular or blocky scandium raw materials with the purity of more than 4N, the aluminum raw materials are granular or blocky aluminum raw materials with the purity of more than 5N, firstly, the scandium raw materials are smelted to obtain scandium melt, then, the granular or blocky aluminum raw materials with the purity of more than 5N are added into the scandium melt to serve as first aluminum raw materials, a first aluminum-scandium alloy is obtained after smelting, then, the granular or blocky aluminum raw materials with the purity of more than 5N are added into the first aluminum-scandium alloy after water cooling, the second aluminum-scandium alloy is obtained after smelting, and a third aluminum raw material is added into the second aluminum-scandium alloy after water cooling according to needs, and smelting is carried out according to the smelting steps to obtain a third aluminum-scandium alloy; adding the aluminum raw material 2-4 times, increasing the smelting frequency to ensure that the melt components are uniform, wherein the amount of the added aluminum raw material does not exceed 60% of the total amount of the aluminum raw material every time, and can be the same or different, so that the method is not particularly limited, relevant parameters of smelting every time are adjusted according to actual needs, and the method is not repeated in the method.
And casting, namely casting the aluminum scandium alloy melt onto a mould for cooling and forming to obtain an aluminum scandium alloy ingot.
The method is characterized in that an aluminum-scandium alloy melt is rapidly cast on a mold for cooling and forming, the casting time is controlled to be 5-10S, the phase of an aluminum-scandium alloy cast ingot can be maintained, the phase splitting phenomenon caused in the slow cooling process is avoided, and the phenomenon that material impurities exceed the standard due to erosion of a crucible caused by the existence of simple substance Al or simple substance Sc can also be effectively avoided.
And melting, namely placing the aluminum-scandium alloy cast ingot in a vacuum crucible furnace, and heating to melt the cast ingot into aluminum-scandium alloy liquid.
And atomizing, namely atomizing the aluminum-scandium alloy liquid to obtain aluminum-scandium alloy powder.
The method comprises the steps of placing an aluminum-scandium alloy ingot in a vacuum crucible, wherein the vacuum crucible furnace is one of an aluminum oxide vacuum crucible furnace, a zirconium oxide vacuum crucible furnace or a magnesium oxide vacuum crucible furnace, a small hole with the size of 5-10 mm is formed in the bottom of the crucible, an atomizing nozzle is installed below the small hole, a plug rod is installed above the small hole and is made of one of aluminum oxide, zirconium oxide or magnesium oxide, the small hole is plugged by the plug rod before atomization begins, a temperature measuring thermocouple is arranged in the crucible, the thermocouple is placed in a protective sleeve and is in contact with alloy liquid, the protective sleeve is preferably made of aluminum oxide, and the thermocouple monitors the temperature of the aluminum-scandium alloy liquid in real time.
Heating the ingot in the crucible to 1450-1650 ℃, keeping the heating time for 25-35 min, melting the ingot in the crucible into aluminum-scandium alloy liquid, then preserving the heat for 5-20 min, controlling the rapid heating to melt the aluminum-scandium alloy ingot into the aluminum-scandium alloy liquid, and enabling the components in the aluminum-scandium alloy liquid to be Al 2 Sc and Al 3 Sc is the main component, no simple substance Al or simple substance Sc exists, so that the aluminum-scandium alloy powder obtained by subsequent atomization powder preparation has uniform granularity, and the phase is Al 2 Sc and Al 3 Sc is used as a main component, no simple substance Al or simple substance Sc phase exists, atomization is carried out after heat preservation is finished, the stopper rod is loosened to enable aluminum-scandium alloy liquid to enter the atomizing nozzle through the small hole to flow out, the aluminum-scandium alloy liquid flows out through the atomizing nozzle to meet gas flowing at a high speed, atomization is carried out to form fine droplets, the droplets are solidified into aluminum-scandium alloy powder in the closed atomizing chamber, the particle size of the obtained aluminum-scandium alloy powder is 20-30 mu m, the oxygen content is less than 2000ppm, the purity is more than 3.5N, and the gas is argon or nitrogenThe pressure of the gas flow is 2-3 MPa.
And sintering, namely sintering the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy target blank.
Placing aluminum-scandium alloy powder in a graphite mold, placing the graphite mold in a hot-pressing sintering furnace, controlling the heating rate to be 10-20 ℃/min, controlling the boosting rate to be 0.5-2 t/min, heating and boosting to the temperature of 950-1150 ℃ and the pressure of 20-40 Mpa, then carrying out constant temperature and constant pressure of 100-240 min, removing the pressure after the constant temperature and constant pressure is finished, cooling the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy powder target blank, when the sintering pressure is more than 40Mpa, cracking of the product is caused by overhigh pressure, the yield of the scandium alloy target material is not favorably improved, the production cost is increased, when the sintering pressure is less than 20Mpa, the density of the target blank is low due to overlow pressure, and the target material has air hole defects.
And (4) machining, namely machining the aluminum-scandium alloy target blank to obtain the aluminum-scandium alloy target.
For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1.
(1) Smelting, namely taking a scandium raw material and an aluminum raw material as reaction raw materials, firstly, suspending the scandium raw material through a cold crucible for smelting to obtain a scandium melt, then adding the aluminum raw material into the scandium melt for smelting for 2 times, adding 45% of the total amount of the aluminum raw material for the first time, adding 55% of the total amount of the aluminum raw material for the second time, and obtaining the aluminum-scandium alloy melt after smelting.
(2) And casting, namely rapidly casting the aluminum scandium alloy melt onto a mould for cooling and forming to obtain the aluminum scandium alloy ingot.
(3) And melting, namely placing the aluminum-scandium alloy cast ingot in a vacuum crucible, heating the cast ingot in the crucible to 1450 ℃, wherein the duration of the heating is 35min, so that the cast ingot in the crucible is melted into aluminum-scandium alloy liquid, and then preserving heat for 5 min.
(4) Atomizing, after heat preservation is finished, enabling the aluminum-scandium alloy liquid to flow into an atomizing nozzle from a small hole at the bottom of the crucible, enabling the aluminum-scandium alloy liquid to flow out through the atomizing nozzle to meet nitrogen with the pressure of gas flow being 2MPa, atomizing into fine droplets, solidifying the droplets into aluminum-scandium alloy powder in a closed atomizing chamber, and obtaining an SEM image of the aluminum-scandium alloy powder in fig. 1. As can be seen from fig. 1, the aluminum-scandium alloy powder is uniform in particle size, and the phase is Al 2 Sc and Al 3 Sc is the main phase, no simple substance Al or simple substance Sc phase exists, and the aluminum-scandium alloy powder has high purity and low oxygen content.
(5) And sintering, namely weighing 300g of aluminum-scandium alloy powder, placing the aluminum-scandium alloy powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, heating to 950 ℃ at the speed of 10 ℃/min, boosting to 20Mpa at the speed of 0.5t/min, then carrying out constant temperature and pressure for 100min, and removing the pressure after the constant temperature and pressure is finished to cool the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy powder target blank.
(6) Machining, taking out the sintered die, demolding and machining to obtain the aluminum-scandium alloy target, testing that the relative density of the target reaches more than 99%, wherein a surface metallographic image before the aluminum-scandium alloy target is corroded is shown in fig. 2, a surface metallographic image after the aluminum-scandium alloy target is corroded is shown in fig. 3, and as can be seen from fig. 2 and 3, the aluminum-scandium target has uniform grain size, and the phase is Al 2 Sc and Al 3 Sc is the main phase, no simple substance Al or simple substance Sc phase exists, and the aluminum-scandium alloy target material has high density.
Example 2.
(1) Smelting, namely taking a scandium raw material and an aluminum raw material as reaction raw materials, firstly, suspending the scandium raw material through a cold crucible for smelting to obtain a scandium melt, then adding the aluminum raw material into the scandium melt for smelting for 4 times, adding 15% of the total amount of the aluminum raw material for the first time, 20% of the total amount of the aluminum raw material for the second time, 30% of the total amount of the aluminum raw material for the third time, and 35% of the total amount of the aluminum raw material for the fourth time, and smelting to obtain the aluminum-scandium alloy melt.
(2) And casting, namely rapidly casting the aluminum scandium alloy melt onto a mould for cooling and forming to obtain the aluminum scandium alloy ingot.
(3) And melting, namely placing the aluminum-scandium alloy cast ingot in a vacuum crucible, heating the cast ingot in the crucible to 1650 ℃, wherein the heating duration is 25min, melting the cast ingot in the crucible into aluminum-scandium alloy liquid, and then preserving heat for 20 min.
(4) And atomizing, wherein after the heat preservation is finished, the aluminum-scandium alloy liquid flows into an atomizing nozzle from a small hole at the bottom of the crucible, the aluminum-scandium alloy liquid flows out through the atomizing nozzle to meet nitrogen with the pressure of gas flow being 3MPa, the aluminum-scandium alloy liquid is atomized into fine droplets, and the droplets are solidified into aluminum-scandium alloy powder in a closed atomizing chamber.
(5) And sintering, namely weighing 300g of aluminum-scandium alloy powder, placing the aluminum-scandium alloy powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, heating to 1150 ℃ at the speed of 20 ℃/min, boosting to 40Mpa at the speed of 2t/min, then carrying out constant temperature and pressure for 240min, and removing the pressure after the constant temperature and pressure are finished so as to obtain the aluminum-scandium alloy powder target blank after the aluminum-scandium alloy powder is cooled.
(6) And (4) machining, namely taking out the sintered die, demolding and machining to obtain the aluminum-scandium alloy target, wherein the relative density of the target is up to more than 99% through testing.
Example 3.
(1) Smelting, namely taking a scandium raw material and an aluminum raw material as reaction raw materials, firstly, suspending the scandium raw material through a cold crucible for smelting to obtain a scandium melt, then adding the aluminum raw material into the scandium melt for 3 times for smelting, wherein the scandium raw material is added into the scandium melt for 25% of the total amount of the aluminum raw material for the first time, the aluminum raw material is added into the scandium melt for the second time, the aluminum raw material is added into the scandium melt for the third time, and the aluminum-scandium alloy melt is obtained after smelting.
(2) And casting, namely rapidly casting the aluminum scandium alloy melt onto a mould for cooling and forming to obtain the aluminum scandium alloy ingot.
(3) And melting, namely placing the aluminum-scandium alloy cast ingot in a vacuum crucible, heating the cast ingot in the crucible to 1450-1650 ℃, wherein the heating duration is 25-35 min, melting the cast ingot in the crucible into aluminum-scandium alloy liquid, and then preserving heat for 5-20 min.
(4) And atomizing, wherein after the heat preservation is finished, the aluminum-scandium alloy liquid flows into an atomizing nozzle from a small hole at the bottom of the crucible, the aluminum-scandium alloy liquid flows out through the atomizing nozzle to meet with nitrogen with the pressure of gas flow being 2.5MPa, the aluminum-scandium alloy liquid is atomized into fine droplets, and the droplets are solidified into aluminum-scandium alloy powder in a closed atomizing chamber.
(5) And sintering, namely weighing 300g of aluminum-scandium alloy powder, placing the aluminum-scandium alloy powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, heating to 1050 ℃ at a speed of 15 ℃/min, boosting to 30Mpa at a speed of 1t/min, then carrying out constant temperature and pressure for 170min, and removing the pressure after the constant temperature and pressure are finished so as to cool the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy powder target blank.
(6) And (4) machining, namely taking out the sintered die, demolding and machining to obtain the aluminum-scandium alloy target, wherein the relative density of the target is up to more than 99% through testing.
According to the preparation method of the aluminum-scandium alloy target, provided by the invention, the aluminum raw material is added into the scandium raw material in batches for smelting according to the characteristic that the metal melting points of aluminum and scandium are greatly different, so that the alloy target can be smelted to be completely alloyed, and the aluminum-scandium alloy powder with high product purity is prepared by adopting a melting and atomizing mode, so that the technical problem that the alloy phase splitting is caused when the aluminum-scandium alloy target is prepared in the prior art is solved.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (2)
1. The preparation method of the aluminum scandium alloy target material is characterized by comprising the following steps:
s1: smelting, namely performing suspension smelting on an aluminum raw material and a scandium raw material through a cold crucible to obtain an aluminum-scandium alloy melt, and specifically comprising the following steps: using a scandium raw material and an aluminum raw material as reaction raw materials, firstly, suspending the scandium raw material through a cold crucible for smelting to obtain a scandium melt, and then adding the aluminum raw material into the scandium melt in batches for smelting to obtain an aluminum-scandium alloy melt;
s2: casting, namely casting the aluminum-scandium alloy melt onto a mold for cooling and forming to obtain an aluminum-scandium alloy ingot, wherein the casting time is 5-10S;
s3: and melting, namely placing the aluminum-scandium alloy cast ingot in a vacuum crucible furnace, heating to melt the cast ingot into aluminum-scandium alloy liquid, and specifically comprising the following steps: placing the aluminum-scandium alloy cast ingot in a vacuum crucible, heating the cast ingot in the crucible to 1450-1650 ℃, wherein the heating duration is 25-35 min, melting the cast ingot in the crucible into aluminum-scandium alloy liquid, and then preserving heat for 5-20 min;
s4: atomizing, namely atomizing the aluminum-scandium alloy liquid to obtain aluminum-scandium alloy powder, and specifically comprising the following steps: enabling the aluminum-scandium alloy liquid to flow out through an atomizing nozzle to meet gas flowing at a high speed, atomizing into fine droplets, and solidifying the droplets into aluminum-scandium alloy powder in a closed atomizing chamber;
s5: sintering, namely sintering the aluminum-scandium alloy powder to obtain an aluminum-scandium alloy target blank, and specifically comprising the following steps: placing the aluminum-scandium alloy powder in a graphite mold, placing the graphite mold in a hot-pressing sintering furnace, raising the temperature and the pressure to 950-1150 ℃, and keeping the pressure at 20-40 Mpa, then carrying out constant temperature and constant pressure for 100-240 min, and removing the pressure after the constant temperature and constant pressure are finished, so that the aluminum-scandium alloy powder is cooled to obtain an aluminum-scandium alloy powder target blank;
s6: machining, namely machining the aluminum-scandium alloy target blank to obtain an aluminum-scandium alloy target;
the specific steps of S3 and S4 are as follows: placing an aluminum scandium alloy ingot in a vacuum crucible, wherein the vacuum crucible furnace is one of an aluminum oxide vacuum crucible furnace, a zirconium oxide vacuum crucible furnace or a magnesium oxide vacuum crucible furnace, a small hole with the size of 5-10 mm is formed in the bottom of the crucible, an atomizing nozzle is installed below the small hole, a stopper rod is installed above the small hole, the stopper rod is made of one of aluminum oxide, zirconium oxide or magnesium oxide, the stopper rod blocks the small hole before atomization begins, a temperature measuring thermocouple is arranged in the crucible, the thermocouple is placed in a protective sleeve and is in contact with alloy liquid, the protective sleeve is made of aluminum oxide, and the thermocouple monitors the temperature of the aluminum scandium alloy liquid in real time; heating the ingot in the crucible to 1450-1650 ℃, keeping the temperature for 25-35 min, melting the ingot in the crucible into aluminum-scandium alloy liquid, then preserving the heat for 5-20 min, controlling the rapid heating to melt the aluminum-scandium alloy ingot into the aluminum-scandium alloy liquid, and enabling the components in the aluminum-scandium alloy liquid to be Al 2 Sc and Al 3 Sc is the main component, no simple substance Al or simple substance Sc exists, the aluminum-scandium alloy powder obtained by subsequent atomization powder preparation has uniform granularity, and the phase is Al 2 Sc and Al 3 The method is characterized in that Sc is used as a main component, no elemental Al or elemental Sc phase exists, atomization is carried out after heat preservation is finished, a stopper rod is loosened to enable aluminum-scandium alloy liquid to enter an atomizing nozzle through a small hole to flow out, the aluminum-scandium alloy liquid flows out through the atomizing nozzle to meet gas flowing at a high speed and is atomized into fine droplets, the droplets are solidified into aluminum-scandium alloy powder in a closed atomizing chamber, the particle size of the obtained aluminum-scandium alloy powder is 20-30 mu m, the oxygen content is less than 2000ppm, the purity is greater than 3.5N, the gas is argon or nitrogen, and the pressure of gas flow is 2-3 MPa.
2. The method according to claim 1, wherein the temperature increase rate in step S5 is 10-20 ℃/min.
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