CN113652657B - Aluminum scandium alloy target material and manufacturing method adopting atmospheric high-temperature diffusion sintering molding - Google Patents
Aluminum scandium alloy target material and manufacturing method adopting atmospheric high-temperature diffusion sintering molding Download PDFInfo
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- CN113652657B CN113652657B CN202110981254.6A CN202110981254A CN113652657B CN 113652657 B CN113652657 B CN 113652657B CN 202110981254 A CN202110981254 A CN 202110981254A CN 113652657 B CN113652657 B CN 113652657B
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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
- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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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
- 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
-
- 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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- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides a manufacturing method of aluminum scandium alloy target atmospheric high-temperature diffusion sintering, which adopts spherical powder raw materials and optimizes the grading of powder granularity, thereby improving the initial apparent density of mixed powder and reducing the gap volume of powder particles; then the powder is filled into a sealed elastic sheath and then subjected to vacuum pumping and ultrahigh pressure cold isostatic pressing, so that the compactness of the formed aluminum scandium biscuit can reach more than 95 percent, which is equivalent to the formation of a layer of sheath skin without penetrating air holes on the surface of the biscuit, the biscuit can be subjected to high-temperature diffusion sintering in an atmosphere sintering furnace without vacuum or inert gas protection, the requirement on equipment performance is greatly reduced, and the process is simple and suitable for large-size and mass production.
Description
Technical Field
The invention relates to the technical field of manufacturing of magnetron sputtering targets, in particular to an atmosphere high-temperature diffusion sintering molding manufacturing method of an aluminum scandium alloy target.
Background
The aluminum-nitrogen-scandium thin film manufactured by reactive sputtering aluminum-scandium alloy target deposition has excellent piezoelectric performance and is widely applied to the fields of micro-electro-mechanical systems (MEMS), radio frequency filters and the like. As the scandium content increased, the piezoelectric constant (d 33 ) Coefficient of electromechanical coupling (kt) 2 ) The piezoelectric performance of the film is more excellent in a linear increase. The aluminum scandium alloy target is usually formed by adopting a smelting process and a powder metallurgy process. The smelting process is relatively simple, but because of the large difference of melting points of aluminum and scandium, the solid solubility of scandium in aluminum is low, the scandium vapor pressure is high, and as the scandium content in the alloy increases, the solid-liquid solidification interval increases, and an intermediate compound phase (Al) is gradually generated 3 Sc、Al 2 Sc、AlSc、AlSc 2 ) The alloy nominal components of the cast ingot are easy to be controlled, the alloy components segregate, the grains are coarse, and the like, so that the subsequent coating components and thickness uniformity are not facilitated. Further, since the brittle intermediate compound phase content in the target material with a high scandium content is large, the ingot plasticity is poor, and it is difficult to perform rolling deformation such as subsequent forging and rolling, and it is difficult to obtain a large-sized aluminum scandium alloy target material, particularly when the scandium content exceeds 20 wt%. In addition, scandium metal has strong activity and is easy to react with a conventional ceramic crucible, so that a water-cooled copper crucible with high cost and high power consumption is generally needed to avoid impurity pollution. The powder metallurgy process can avoid the problems of segregation of alloy components, coarse grains and the like in the smelting process, and can be formed in a large size. The hot-press or hot isostatic pressing sintering molding is commonly used, but special vacuum or inert gas protection sintering equipment is needed, a hot-press molding die is easy to damage, a metal package used for hot isostatic pressing is disposable, the target material molding cost is high, and the productivity is low.
Disclosure of Invention
The invention aims to provide a brand-new manufacturing method of atmospheric high-temperature diffusion sintering molding of aluminum scandium alloy target material, which adopts spherical powder raw materials and optimizes the grading of powder granularity, thereby improving the initial apparent density of mixed powder and reducing the gap volume of powder particles; then the powder is filled into a sealed elastic sheath and then subjected to vacuum pumping and ultrahigh pressure cold isostatic pressing, so that the compactness of the formed aluminum scandium biscuit can reach more than 95 percent, which is equivalent to the formation of a layer of sheath skin without penetrating air holes on the surface of the biscuit, the biscuit can be subjected to high-temperature diffusion sintering in an atmosphere sintering furnace without vacuum or inert gas protection, the requirement on equipment performance is greatly reduced, and the process is simple and suitable for large-size and mass production. On the other hand, because the powder is subjected to high vacuum exhaust treatment before cold isostatic pressing treatment, the inside of the biscuit is a closed gap and is approximately vacuum, so that the increment of gas impurities in the aluminum scandium alloy target is extremely low, the high purity of the aluminum scandium target is realized, the densification moving resistance among particles in the diffusion sintering process is low, and the high-density molding of the aluminum scandium target is facilitated.
In order to solve the technical problems, the invention provides a manufacturing method for atmospheric high-temperature diffusion sintering molding of an aluminum scandium alloy target, which comprises the following steps:
firstly, selecting spherical Al metal powder and Sc metal powder with optimized grain size grading as raw materials, and carrying out batching and uniform mixing according to target alloy components;
step two, filling the mixed powder obtained in the step one into a closed elastic sheath, and performing cold isostatic pressing to obtain an aluminum scandium biscuit;
thirdly, placing the aluminum scandium biscuit into an atmosphere sintering furnace for diffusion sintering to obtain an aluminum scandium alloy target blank;
and fourthly, machining the aluminum scandium alloy target blank obtained in the third step, and welding the aluminum scandium alloy target blank with a backboard to obtain a finished product of the aluminum scandium alloy target material.
The particle size distribution of the spherical powder in the first step is as follows: d10 is 5-10 μm, D50 is 40-80 μm, and D90 is 100-150 μm.
The bulk density of the powder in the second step is more than 50%.
The third step is that the elastic sheath is vacuumized to be smaller than 1.3 x 10 -4 Pa, the pressure of static pressure forming is preferably 500-700 MPa, the dwell time is preferably 5-10 min, and the density of the obtained aluminum scandium alloy target blank is more than 95%.
In the fourth step, the diffusion sintering temperature is preferably 500-630 ℃, the diffusion sintering time is preferably 6-12 hours, and the density of the obtained aluminum scandium alloy target blank is more than 99%.
The scandium mass content in the aluminum scandium alloy target material is preferably 5-55wt%.
The beneficial effects of the invention are that
1. The invention discloses an atmospheric high-temperature diffusion sintering molding manufacturing method of an aluminum scandium alloy target, which adopts spherical powder raw materials and optimizes the grading of the granularity of the powder, thereby improving the bulk density of mixed powder, reducing the gap volume of the powder particles, and vacuumizing after the powder is filled into a closed elastic sheath to be better than 1.3 x 10 -4 Pa, the density of aluminum scandium biscuit with more than 95% obtained by cold isostatic pressing, wherein the inside of the biscuit is a closed gap and is approximately vacuum, on the one hand, in the subsequent diffusion sintering process, equipment does not need vacuum or inert gas protection, the surface of the blank does not need metal sheath isolation, the extremely low increment of gas impurities in the aluminum scandium alloy target can be achieved, and gas impurities in a sintering furnace cannot permeate into the target blank, so that the high purity of the aluminum scandium target is realized; on the other hand, the closed gaps in the biscuit are approximately vacuum, and the inter-particle densification moving resistance in the diffusion sintering process is low, so that the high-densification forming of the aluminum scandium target material is facilitated.
2. According to the atmospheric high-temperature diffusion sintering molding manufacturing method of the aluminum scandium alloy target, the biscuit is molded at room temperature, the high-temperature diffusion sintering temperature is lower than the melting point of aluminum, and the raw materials do not flow and burn and volatilize in the whole target molding process, so that the uniformity of components of the aluminum scandium alloy target and the accuracy of components of the alloy are ensured. In addition, the conventional cold isostatic pressing furnace and the atmospheric sintering furnace are adopted, the process is simple and controllable, and the high-efficiency production with large size and large batch is easy, and the cost is low.
Drawings
FIG. 1 is a flow chart of a method for manufacturing an aluminum scandium alloy target according to the present invention.
Detailed Description
The invention provides a manufacturing method for atmospheric high-temperature diffusion sintering molding of an aluminum scandium alloy target, which comprises the following steps:
firstly, selecting spherical Al metal powder and Sc metal powder with optimized grain size grading as raw materials, and carrying out batching and uniform mixing according to target alloy components;
step two, filling the mixed powder obtained in the step one into a closed elastic sheath, and performing cold isostatic pressing to obtain an aluminum scandium biscuit;
thirdly, placing the aluminum scandium biscuit into an atmosphere sintering furnace for diffusion sintering to obtain an aluminum scandium alloy target blank;
and fourthly, machining the aluminum scandium alloy target blank obtained in the third step, and welding the aluminum scandium alloy target blank with a backboard to obtain a finished product of the aluminum scandium alloy target material.
The particle size distribution of the spherical powder in the first step is as follows: d10 is 5-10 μm, D50 is 40-80 μm, and D90 is 100-150 μm. With this particle size distribution it is possible to achieve filling of the large ball powder interstices with small ball powder to increase the bulk density, which would not be too high if the particle size was too fine or too coarse.
The bulk density of the powder in the second step is more than 50%.
The third step is that the elastic sheath is vacuumized to be smaller than 1.3 x 10 -4 Pa, the pressure of static pressure forming is preferably 500-700 MPa, the dwell time is preferably 5-10 min, and the density of the obtained aluminum scandium alloy target blank is more than 95%.
In the fourth step, the diffusion sintering temperature is preferably 500-630 ℃, the diffusion sintering time is preferably 6-12 hours, and the density of the obtained aluminum scandium alloy target blank is more than 99%.
The scandium mass content in the aluminum scandium alloy target material is preferably 5-55wt%.
The following examples are used to describe embodiments of the present invention in detail, so that the technical means can be applied to the present invention to solve the technical problems, and the implementation process for achieving the technical effects can be fully understood and implemented accordingly.
1. Mixing ingredients
According to the nominal aluminum scandium alloy target material composition designed in the embodiment, raw material proportioning and mixing are carried out:
the raw materials are spherical Al metal powder and Sc metal powder, and the particle size distribution of the powder is as follows: d10 is 5-10 μm, D50 is 40-80 μm, and D90 is 100-150 μm. Mixing the initial powder uniformly by adopting V-shaped double-cone powder mixing machines to obtain mixed powder, wherein the scandium mass content is 5-55wt%, and the bulk density of the mixed powder is more than 50%.
2. Cold isostatic pressing
Filling the mixed powder into a sealed elastic sheath, and vacuumizing the elastic sheath by adopting an oil diffusion pump or a molecular pump to be better than 1.3 x 10 -4 Pa, then carrying out cold isostatic compaction on the powder along with an elastic sheath, wherein the pressure is 500-700 MPa, and the pressure maintaining time is 5-10 min. And removing the elastic sheath to obtain the aluminum scandium biscuit with the density of more than 95%.
3. High temperature diffusion sintering
And (3) placing the aluminum scandium alloy blank in an atmosphere thermal sintering furnace for diffusion sintering, wherein the diffusion sintering temperature is 500-630 ℃, and the diffusion sintering time is 6-12 hours, so that the aluminum scandium alloy target blank with the density of more than 99% is obtained.
4. Machining welding
And (3) machining the aluminum-scandium alloy target blank, and welding the aluminum-scandium alloy target blank with the backboard to obtain the finished product aluminum-scandium alloy target.
The main manufacturing processes and the performance results of the aluminum scandium alloy targets of examples 1 to 10 and comparative examples 1 to 6 are shown in Table 1.
TABLE 1 aluminium scandium alloy target manufacturing process and performance results
It can be seen from the examples and comparative examples in Table 1 that when the powder size fraction is not sufficiently optimized, the bulk density of the mixed powder is less than 50%, as in comparative examples 1 to 6; or the vacuum degree difference of the sheath is less than 1.3 x 10 -4 Pa, such as comparative examples 1, 2, 5 and 6, causes excessive gap volume of powder particles and excessive residual gas among gaps, thereby reducing aluminum scandium biscuit and final sintering density, and being difficult to reach more than 99%.
By adopting spherical powder raw materials and carrying out optimized grading on the powder granularity, the initial loose packing density of the mixed powder is improved, and the gap volume of powder particles is reduced; then the powder is filled into a sealed elastic sheath and then is subjected to vacuum pumping and ultrahigh pressure cold isostatic pressing, so that the compactness of the formed aluminum scandium biscuit can reach more than 95 percent, which is equivalent to the formation of a layer of sheath skin without penetrating air holes on the surface of the biscuit, and the biscuit can be subjected to high-temperature diffusion sintering in an atmosphere sintering furnace without vacuum or inert gas protection.
All of the above-described primary implementations of this intellectual property are not intended to limit other forms of implementing this new product and/or new method. Those skilled in the art will utilize this important information and the above modifications to achieve a similar implementation. However, all modifications or adaptations belong to the reserved rights based on the new products of the invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (5)
1. The method for manufacturing the aluminum scandium alloy target material by high-temperature diffusion sintering and forming in the atmosphere is characterized by comprising the following steps of:
firstly, selecting spherical Al metal powder and Sc metal powder with optimized grain size distribution as raw materials, and carrying out batching and uniform mixing according to target alloy components, wherein the grain size distribution of the spherical powder in the first step is as follows: d10 is 5-10 mu m, D50 is 40-80 mu m, D90 is 100-150 mu m, and the loose powder density is more than 50%;
the second step, the mixed powder obtained in the first step is filled into a sealed elastic sheath, and the vacuum of the elastic sheath is superior to that of the elastic sheath with the pressure of 1.3 multiplied by 10 -4 Pa, cold isostatic compaction, wherein the static compaction pressure is 500-700 MPa, the dwell time is 5-10 min, and the aluminum scandium biscuit with the density of more than 95% is obtained;
thirdly, placing the aluminum scandium biscuit into an atmosphere sintering furnace for diffusion sintering to obtain an aluminum scandium alloy target blank;
and fourthly, machining the aluminum scandium alloy target blank obtained in the third step, and welding the aluminum scandium alloy target blank with a backboard to obtain a finished product of the aluminum scandium alloy target material.
2. The method for manufacturing the aluminum scandium alloy target material by high-temperature diffusion sintering and forming in the atmosphere is characterized in that: the diffusion sintering temperature in the third step is 500-630 ℃, and the diffusion sintering time is 6-12 hours.
3. The method for manufacturing the aluminum scandium alloy target material by atmospheric high temperature diffusion sintering according to claim 1 or 2, which is characterized in that: and the compactness of the aluminum scandium alloy target blank obtained in the third step is more than 99%.
4. An aluminum scandium alloy target manufactured by the manufacturing method according to any one of claims 1 to 3.
5. The aluminum scandium alloy target according to claim 4, wherein: scandium content is 5-55wt%.
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