CN113061852B - High-purity aluminum or aluminum alloy target material and preparation method thereof - Google Patents
High-purity aluminum or aluminum alloy target material and preparation method thereof Download PDFInfo
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- CN113061852B CN113061852B CN202110287178.9A CN202110287178A CN113061852B CN 113061852 B CN113061852 B CN 113061852B CN 202110287178 A CN202110287178 A CN 202110287178A CN 113061852 B CN113061852 B CN 113061852B
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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
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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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 invention provides a high-purity aluminum or aluminum alloy target material and a preparation method thereof, wherein the preparation method comprises the following steps: sequentially carrying out forging and stretching, primary heat treatment, forging, secondary heat treatment, rolling and tertiary heat treatment on the aluminum or aluminum alloy target blank to obtain a high-purity aluminum or aluminum alloy target; the rolling passes are 3-5 times; the pressure drop of the rolling is reduced along with the pass; the preparation method obviously refines the grain size and improves the uniformity of the grains by optimizing the rolling process, has simple process flow and low cost, is beneficial to large-scale production and has better industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of liquid crystal target preparation, and particularly relates to a high-purity aluminum or aluminum alloy target and a preparation method thereof.
Background
Physical Vapor Deposition (PVD) is one of the most critical processes in the production process of semiconductor chips and TFT-LCDs, the sputtering metal target material for PVD is one of the most important raw materials in the production process of semiconductor chips and the preparation and processing process of TFT-LCDs, and the sputtering metal target material with the largest consumption is high-purity aluminum and high-purity aluminum alloy target materials. According to the principle of the sputtering process, the finer the crystal grains of the target material, the more uniform the component structure, and the smaller the surface roughness of the target material, the better the quality of the film formed on the silicon wafer by the physical vapor deposition method, so that the size of the crystal grains of the target material is particularly important to be refined. The grain size of the high-purity aluminum target material is less than 200 μm. However, as is clear from the solidification characteristics of pure metals, the higher the purity and the higher the cleanliness of the metal, the smaller the probability of heterogeneous nucleation during solidification, the more likely the grains formed by solidification grow, and the more likely the grains grow as cellular crystals along the preferential growth surface, and the minimum grain size of the high purity aluminum grain refined by controlling the solidification process can only reach 2mm diameter. Therefore, the search for a new process to refine the grain size is a problem that needs to be solved urgently.
CN110205590A discloses an ultra-high purity aluminum sputtering target material and a preparation method thereof, in the rolling process, the roll gap of a rolling mill is set to be half of single-pass reduction to roll ultra-high purity aluminum cast ingots, the rolled ultra-high purity aluminum cast ingots are rewound after being bitten, the roll gap is set to be single-pass reduction to roll the ultra-high purity aluminum cast ingots again, so that the phenomenon of biting and slipping in the rolling process is avoided, and the rolling with large reduction is realized. The method can obtain qualified finished products only by rolling for multiple times, and has low production efficiency.
CN101638760A discloses a preparation method of an ultra-pure aluminum ultra-fine grain sputtering target material in the technical field of metal material processing, which comprises the following steps: placing the ultra-pure aluminum plate in an equal-channel angular extrusion die to carry out extrusion treatment for 3 to 15 passes; carrying out deep supercooling treatment on the ultra-high purity aluminum plate obtained after extrusion in a liquid nitrogen environment, wherein the deep supercooling temperature is-80 ℃ to-10 ℃; and (4) rolling the ultra-high purity aluminum plate subjected to deep undercooling treatment for 3-15 rolling passes. The preparation method has complex working procedures, the extrusion treatment and the rolling are carried out for many times, and the production efficiency is lower; and low-temperature treatment is also needed, so that the cost is increased, and the large-scale production is not facilitated.
In conclusion, how to provide a method for refining the grain size of high-purity aluminum and high-purity aluminum alloy target materials, which has simple process and low cost, becomes a problem to be solved urgently at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high-purity aluminum or aluminum alloy target material and a preparation method thereof, wherein the preparation method obviously refines the grain size and improves the uniformity of grains by optimizing a rolling process; the preparation method has the advantages of simple process flow, low cost, contribution to large-scale production and better industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a preparation method of a high-purity aluminum or aluminum alloy target material, which comprises the following steps:
sequentially carrying out forging and stretching, primary heat treatment, forging, secondary heat treatment, rolling and tertiary heat treatment on the aluminum or aluminum alloy target blank to obtain a high-purity aluminum or aluminum alloy target;
the rolling passes are 3-5 times, such as 3 times, 4 times or 5 times;
the pressure drop of the rolling is reduced along with the pass.
According to the preparation method, the rolling process is optimized, the secondary pressure drop of each pass is adjusted, the rolling passes are reduced, and the production efficiency is improved; the preparation method can improve the grain uniformity of the target by only rolling for at most 3-5 times, obviously reduces energy consumption compared with a process of homogenizing grains by increasing the heat treatment temperature, reduces production cost compared with a process of rolling for multiple times, improves the utilization rate of the target, and has better industrial application prospect.
In the invention, the rolling direction is to roll along the length direction of the aluminum or aluminum alloy target blank, namely the reduction in the height direction.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
In a preferred embodiment of the present invention, the aluminum or aluminum alloy target blank is cut before being forged and stretched.
Preferably, the cut aluminum or aluminum alloy target blank is a cuboid.
Preferably, the rectangular parallelepiped has dimensions of (245 to 250mm) × (290 to 295mm), for example 245mm × 245mm × 290mm, 248mm × 248mm × 293mm, 250mm × 250mm × 292mm, 246mm × 246mm × 295mm, 245mm × 245mm × 295mm, and the like, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
In the invention, the size of the cut aluminum or aluminum alloy target blank can be determined according to the requirement of the finally required target, and the finally required target is used in the field of LCD, so that the finally obtained target has larger size.
As a preferred embodiment of the present invention, the forging and drawing are preheated before the forging and drawing.
Preferably, the temperature of the preheating is 140 to 160 ℃, for example, 140 ℃, 145 ℃, 150 ℃, 155 ℃ or 160 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the preheating time is 10-15 min, such as 10min, 11min, 12min, 13min, 14min or 15min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the dimensions of the wrought aluminum or aluminum alloy target blank are (298-302 mm) × (198-202 mm), such as 298mm × 298mm × 198mm, 300mm × 300mm × 200mm, 302mm × 302mm × 202mm, 299mm × 299mm × 200mm, or 301mm × 301mm × 201mm, but are not limited to the recited values, and other values not recited in the range of values are also applicable.
In the present invention, large grains formed during casting of the raw material can be destroyed by forging and drawing.
In a preferred embodiment of the present invention, the temperature of the primary heat treatment is 295 to 305 ℃, for example 295 ℃, 297 ℃, 300 ℃, 303 ℃ or 305 ℃, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the time of the primary heat treatment is 58 to 62min, such as 58min, 59min, 60min, 61min or 62min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the invention, the crystal grains of the material structure can be fully grown by one-time heat treatment.
In a preferred embodiment of the present invention, the forging is performed by preheating.
Preferably, the temperature of the preheating is 140 to 160 ℃, for example, 140 ℃, 145 ℃, 150 ℃, 155 ℃ or 160 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the preheating time is 10-15 min, such as 10min, 11min, 12min, 13min, 14min or 15min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the dimensions of the forged aluminum or aluminum alloy target blank are (765-770 mm) × (188-192 mm) × (120-125 mm), such as 768mm × 190mm × 123mm, 765mm × 188mm × 120mm, 769mm × 192mm × 125mm, 765mm × 192mm × 123mm, or 770mm × 191mm × 124mm, but the invention is not limited to the values listed, and other values not listed in the numerical range are also applicable.
In the present invention, the blank can be given the desired shape and dimensions by forging.
In a preferred embodiment of the present invention, the temperature of the secondary heat treatment is 290 to 310 ℃, for example 290 ℃, 295 ℃, 300 ℃, 305 ℃ or 310 ℃, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the time of the secondary heat treatment is 25 to 40min, such as 25min, 30min, 35min or 40min, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
According to the invention, the temperature of the metal workpiece in the subsequent rolling process can be ensured through secondary heat treatment, and the material is softened at the same time, so that the rolling process is ensured.
In a preferred embodiment of the present invention, the temperature of the first pass of the rolling is 295 to 305 ℃, for example 295 ℃, 297 ℃, 300 ℃, 302 ℃ or 305 ℃, but the temperature is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the rolling passes are 3.
Preferably, the reduction amount in the first pass of the rolling is 30 to 52mm, for example, 30mm, 35mm, 40mm, 45mm, 48mm, 49mm, 50mm, 51mm, or 52mm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, and preferably 48 to 52 mm.
Preferably, the reduction in the second pass of the rolling is 20 to 42mm, for example 20mm, 25mm, 30mm, 35mm, 38mm, 39mm, 40mm, 41mm or 42mm, but is not limited to the values listed, and other values not listed within this range are equally applicable, preferably 38 to 42 mm.
Preferably, the reduction in the third pass of the rolling is 8 to 20mm, for example 8mm, 9mm, 10mm, 11mm, 12mm, 15mm, 17mm or 20mm, but is not limited to the recited values, and other values within this range are equally applicable, preferably 8 to 12 mm.
Preferably, the reduction in the fourth pass of the rolling is 5 to 10mm, for example 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, but not limited to the values listed, and other values not listed within this range are equally applicable.
Preferably, the rolling reduction in the fifth pass is 5 to 10mm, for example 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, but is not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, the total rolling reduction is 98-102 mm, such as 98mm, 99mm, 100mm, 101mm or 102mm, but not limited to the recited values, and other values not recited within the range of values are also applicable.
In the invention, the pressure drop of each rolling has certain influence on the properties of the finally obtained target material. If the pressure drop is too small, the tissues of all the areas can not be completely deformed, and large grains can not be crushed, so that the uniformity is influenced; if the pressure drop is too large, the local stress is too large, the tissue is extruded, the original crystal grains can be phagocytosed by partial crystal grains, small crystal grains can grow out in the crystal grains of large grains in the subsequent recrystallization process, in addition, due to the large pressure, the brittleness of the material can be shown, microcracks can easily appear in the material, and the abnormal discharge in the use process is caused.
Preferably, the temperature after rolling is normal temperature.
And leveling after rolling.
Preferably, the flattened bow is no greater than 1mm, such as 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, or 1mm, but is not limited to the recited values, and other values within the range are equally applicable.
In a preferred embodiment of the present invention, the temperature of the third heat treatment is 245 to 255 ℃, for example, 245 ℃, 248 ℃, 250 ℃, 252 ℃ or 255 ℃, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the time of the third heat treatment is 13-17 min, such as 13min, 14min, 15min, 16min or 17min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the present invention, the purpose of the three heat treatments is to recrystallize the metal material to produce a desired grain size.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) cutting to obtain aluminum or aluminum alloy target blanks with the sizes of (290-295 mm) × (245-250 mm); preheating the obtained aluminum or aluminum alloy target blank at the temperature of 140-160 ℃ for 10-15 min, and then forging and stretching, wherein the size of the forged and stretched aluminum or aluminum alloy target blank is (198-202 mm) × (298-302 mm);
(2) carrying out primary heat treatment at 295-305 ℃ for 58-62 min;
(3) preheating for 10-15 min at the temperature of 140-160 ℃, and then forging, wherein the size of the forged aluminum or aluminum alloy target blank is (765-770 mm) × (188-192 mm) × (120-125 mm);
(4) carrying out secondary heat treatment at 290-310 ℃ for 25-40 min;
(5) rolling for 3-5 times, wherein the pressure drop of the first pass is 30-52 mm, the pressure drop of the second pass is 20-42 mm, the pressure drop of the third pass is 20-42 mm, the pressure drop of the fourth pass is 5-10 mm, the pressure drop of the fifth pass is 5-10 mm, and the total pressure drop is 98-102 mm; leveling after rolling, wherein the curvature after leveling is not more than 1 mm;
(6) and carrying out three times of heat treatment at 245-255 ℃ for 13-17 min to obtain the high-purity aluminum or aluminum alloy target material.
In another aspect, the present invention provides a high purity aluminum or aluminum alloy target material prepared by the above preparation method, wherein the purity of the high purity aluminum or aluminum alloy target material is 5N-5N 5, such as 99.999%, 99.9991%, 99.9992%, 99.9993%, 99.9994% or 99.9995%, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the maximum grain size of the high-purity aluminum or aluminum alloy target material is not more than 200 μm, such as 140 μm, 150 μm, 160 μm, 170 μm, 180 μm, 190 μm, or 200 μm, but is not limited to the recited values, and other unrecited values within the range of values are also applicable.
In the invention, the high-purity aluminum or aluminum alloy target is applied to the field of liquid crystal, and the grain size of the high-purity aluminum or aluminum alloy target is not more than 200 mu m.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the preparation method, the rolling process is optimized, the target crystal grains can be refined only by rolling for 3-5 times, the uniformity of the target crystal grains is remarkably improved, and the obtained target crystal grains are all below 200 mu m and the average grain diameter is all below 150 mu m by further controlling the pressure drop of the internal rolling;
(2) compared with the process of homogenizing crystal grains by increasing the heat treatment temperature, the preparation method provided by the invention has the advantages that the energy consumption is obviously reduced, compared with the process of rolling for multiple times, the production cost is reduced, the production efficiency is improved, the utilization rate of the target material is improved, and the industrial application prospect is better.
Drawings
FIG. 1 is an electron back-scattered diffraction (EBSD) chart of a high purity aluminum target provided in example 3 of the present invention;
fig. 2 is an Electron Back Scattering Diffraction (EBSD) diagram of the high purity aluminum target provided in example 6 of the present invention.
Detailed Description
In order to better explain the present invention and to facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical, but non-limiting, examples of the present invention:
example 1:
the embodiment provides a preparation method of a high-purity aluminum target, which comprises the following steps:
(1) cutting to obtain aluminum target blanks with the dimensions of 290mm multiplied by 245 mm; preheating the obtained aluminum target blank at the temperature of 140 ℃ for 10min, and then performing forging and stretching, wherein the size of the forged and stretched aluminum target blank is 198mm multiplied by 298 mm;
(2) carrying out primary heat treatment at 295 ℃ for 58 min;
(3) preheating for 10min at the temperature of 140 ℃, and then forging, wherein the size of the forged aluminum target blank is 765mm multiplied by 188mm multiplied by 120 mm;
(4) performing secondary heat treatment at 310 deg.C for 25 min;
(5) rolling for 3 times, wherein the reduction amount of the first pass is 50mm, the reduction amount of the second pass is 40mm, and the reduction amount of the third pass is 10 mm; leveling after rolling, wherein the curvature after leveling is 1 mm;
(6) and carrying out heat treatment for three times at 255 ℃ for 13min to obtain the high-purity aluminum target material.
Example 2:
the embodiment provides a preparation method of a high-purity aluminum-silicon alloy target, and the adopted blank mainly comprises the following components: 99 wt% of aluminum and 1 wt% of Si.
The preparation method comprises the following steps:
(1) cutting to obtain aluminum-silicon alloy target blanks with the sizes of 295mm multiplied by 250 mm; preheating the obtained aluminum-silicon alloy target blank at the temperature of 160 ℃ for 15min, and then performing forging and stretching, wherein the size of the forged aluminum-silicon alloy target blank is 202mm multiplied by 302 mm;
(2) performing primary heat treatment at 305 deg.C for 62 min;
(3) preheating for 15min at the temperature of 160 ℃, and then forging, wherein the size of the forged aluminum-silicon alloy target blank is 770mm multiplied by 192mm multiplied by 125 mm;
(4) performing secondary heat treatment at 290 deg.C for 40 min;
(5) rolling for 3 times, wherein the pressure drop of the first pass is 48mm, the pressure drop of the second pass is 42mm, and the pressure drop of the third pass is 12 mm; leveling after rolling, wherein the curvature after leveling is 0.9 mm;
(6) and carrying out heat treatment for three times at 245 ℃ for 17min to obtain the high-purity aluminum-silicon alloy target material.
Example 3:
the embodiment provides a preparation method of a high-purity aluminum target, which comprises the following steps:
(1) cutting to obtain aluminum target blanks with the sizes of 293mm multiplied by 248 mm; preheating the obtained aluminum target blank at the temperature of 150 ℃ for 12min, and then performing forging and stretching, wherein the size of the forged and stretched aluminum target blank is 200mm multiplied by 300 mm;
(2) performing primary heat treatment at 300 deg.C for 60 min;
(3) preheating for 13min at the temperature of 150 ℃, and then forging, wherein the size of the forged aluminum target blank is 768mm multiplied by 190mm multiplied by 123 mm;
(4) performing secondary heat treatment at 300 deg.C for 30 min;
(5) rolling for 3 times, wherein the pressure drop of the first pass is 52mm, the pressure drop of the second pass is 38mm, and the pressure drop of the third pass is 8 mm; leveling after rolling, wherein the curvature after leveling is 1 mm;
(6) and carrying out heat treatment for three times at 250 ℃ for 15min to obtain the high-purity aluminum target.
As shown in fig. 1, the EBSD pattern of the high purity aluminum target obtained by the production method of the present example is shown in fig. 1, and it is understood from fig. 1 that the high purity aluminum target obtained does not have significantly abnormal coarse grains, and microscopically does not have the presence of recrystallized small grains among the large grains, nor elongated coarse grains.
Example 4:
the embodiment provides a preparation method of a high-purity aluminum target, which comprises the following steps:
(1) cutting to obtain an aluminum target blank having a size of 292mm × 245mm × 245 mm; preheating the obtained aluminum target blank at the temperature of 145 ℃ for 12min, and then performing forging and stretching, wherein the size of the forged and stretched aluminum target blank is 199mm multiplied by 299 mm;
(2) performing primary heat treatment at 302 deg.C for 60 min;
(3) preheating for 15min at the temperature of 148 ℃, and then forging, wherein the size of the forged aluminum target blank is 769mm × 191mm × 124 mm;
(4) performing secondary heat treatment at 300 deg.C for 35 min;
(5) rolling for 5 times, wherein the reduction amount of the first pass is 50mm, the reduction amount of the second pass is 30mm, the reduction amount of the third pass is 10mm, the reduction amount of the fourth pass is 5mm, and the reduction amount of the fifth pass is 5 mm; leveling after rolling, wherein the curvature after leveling is 0.8 mm;
(6) and carrying out heat treatment for three times at 248 ℃ for 14min to obtain the high-purity aluminum target.
Example 5:
the present embodiment provides a method for preparing a high-purity aluminum alloy target, wherein an aluminum alloy target blank is used as the aluminum-silicon alloy target blank used in embodiment 2.
The preparation process is referred to the preparation process in example 2, with the only difference that: and (3) in the step (5), the pressure drop amount of the first pass is 40mm, and the reduced pressure drop amount is proportionally increased to the second pass and the third pass respectively, namely the pressure drop amount of the second pass is 48.2mm, and the pressure drop amount of the third pass is 13.8 mm.
Example 6:
this embodiment provides a method for preparing a high-purity aluminum target, and the aluminum target blank used in embodiment 3 is the aluminum target blank.
The preparation is referred to the preparation in example 3, differing only in that: in the step (5), the pressure drop amount of the first pass is 60mm, the increased pressure drop amount is respectively reduced by the pressure drop amount of the second pass rolling and the pressure drop amount of the third pass rolling according to proportion, namely the pressure drop amount of the second pass is 31.4mm, and the pressure drop amount of the third pass is 6.6 mm.
The EBSD diagram of the high purity aluminum target obtained by the preparation method of this embodiment is shown in fig. 2, and it can be known from fig. 2 that the obtained high purity aluminum target has poor structural uniformity, a large recrystallized small grain structure and an incompletely crystallized structure exist in a large grain, and a flaky molten large grain appears.
Example 7:
the embodiment provides a preparation method of a high-purity aluminum alloy target, and the adopted aluminum alloy target blank is the aluminum-silicon alloy target blank used in the embodiment 2.
The preparation is referred to the preparation in example 2, differing only in that: and (5) reducing the pressure reduction amount of the second pass in the step (5) to 50mm, wherein the increased pressure reduction amount is reduced by the pressure reduction amount of the first pass and the pressure reduction amount of the third pass respectively according to a proportion, namely the pressure reduction amount of the first pass is 41.6mm, and the pressure reduction amount of the third pass is 10.4 mm.
Example 8:
this embodiment provides a method for preparing a high-purity aluminum target, and the aluminum target blank used in embodiment 3 is the aluminum target blank.
The preparation process is referred to the preparation process in example 3, with the only difference that: and (3) in the step (5), the pressure drop amount of the second pass is 30mm, the reduced pressure drop amount is proportionally increased to the pressure drop amount of the first pass and the pressure drop amount of the third pass respectively, namely the pressure drop amount of the first pass is 58.9mm, and the pressure drop amount of the third pass is 9.1 mm.
Example 9:
the present embodiment provides a method for preparing a high-purity aluminum alloy target, wherein an aluminum alloy target blank is used as the aluminum-silicon alloy target blank used in embodiment 2.
The preparation process is referred to the preparation process in example 2, with the only difference that: and (3) in the step (5), the pressure drop of the third pass is 18mm, the increased pressure drop is proportionally reduced by the pressure drop of the first pass and the pressure drop of the second pass, namely the pressure drop of the first pass is 44.8mm, and the pressure drop of the second pass is 39.2 mm.
Example 10:
this embodiment provides a method for preparing a high-purity aluminum target, and the aluminum target blank used in embodiment 3 is the aluminum target blank.
The preparation process is referred to the preparation process in example 3, with the only difference that: and (5) the pressure drop of the third pass in the step (5) is 4mm, the reduced pressure drop is increased to the pressure drop of the first pass and the second pass in proportion, namely the pressure drop of the first pass is 54.3mm, and the pressure drop of the second pass is 39.7 mm.
The maximum grain size, average grain size, minimum grain size, and purity of the high purity aluminum targets or aluminum alloy targets obtained in examples 1 to 10 were measured, and the results are shown in table 1.
TABLE 1 maximum grain size, average grain size, minimum grain size and purity of the high purity aluminum or aluminum alloy targets obtained in examples 1-10
In the embodiments 1 to 4, by optimizing the rolling process and adjusting the pressure drop amount of each pass, the average grain size of the obtained high-purity aluminum or aluminum alloy target material can be reduced to below 150 μm only by rolling for 3 to 5 times, and the maximum grain size is not more than 200 μm.
In the embodiment 5-10, the pressure drop of one pass of rolling is reduced or increased in the preparation process, so that the uniformity of the obtained high-purity aluminum or aluminum alloy target material is poor, and the reduction of the pressure drop can prevent the tissues of all areas from being completely deformed, prevent large grains from being crushed and influence the uniformity; the increase of the pressure drop can cause the local stress to be overlarge, the structure is extruded, the original crystal grains can be eaten by partial crystal grains, and in the subsequent recrystallization process, small crystal grains can grow out from the large-grain crystal grains.
The preparation method provided by the invention has the advantages that the rolling process is optimized, the secondary pressure drop of each pass is adjusted, the rolling passes are reduced, and the production efficiency is improved; the preparation method can improve the grain uniformity of the target by rolling for 3-5 times, obviously reduces energy consumption compared with a process of homogenizing grains by increasing the heat treatment temperature, reduces production cost compared with a process of rolling for multiple times, improves the utilization rate of the target, and has better industrial application prospect.
The applicant states that the present invention is illustrated by the above examples to show the products and detailed methods of the present invention, but the present invention is not limited to the above products and detailed methods, i.e. it is not meant that the present invention must rely on the above products and detailed methods to be carried out. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (29)
1. The preparation method of the high-purity aluminum or aluminum alloy target is characterized by comprising the following steps of:
sequentially carrying out forging and stretching, primary heat treatment, forging, secondary heat treatment, rolling and tertiary heat treatment on the aluminum or aluminum alloy target blank to obtain a high-purity aluminum or aluminum alloy target;
the rolling passes are 3-5 times;
the pressure drop of the rolling is reduced along with the pass;
the pressure drop of the first pass of rolling is 48-52 mm;
the pressure drop of the second pass of rolling is 38-42 mm;
and the pressure drop of the third pass of rolling is 8-12 mm.
2. The method according to claim 1, wherein the aluminum or aluminum alloy target blank is cut before forging.
3. The method according to claim 2, wherein the cut aluminum or aluminum alloy target blank is a rectangular parallelepiped.
4. The method according to claim 3, wherein the rectangular parallelepiped has a size of (245 to 250mm) x (290 to 295 mm).
5. The method of claim 1, wherein the pre-heating is performed prior to the forging.
6. The method according to claim 5, wherein the preheating temperature is 140 to 160 ℃.
7. The preparation method according to claim 5, wherein the preheating time is 10-15 min.
8. The method according to claim 1, wherein the dimensions of the wrought aluminum or aluminum alloy target blank are (298-302 mm) × (198-202 mm).
9. The method according to claim 1, wherein the temperature of the primary heat treatment is 295-305 ℃.
10. The method according to claim 1, wherein the time of the primary heat treatment is 58 to 62 min.
11. The method of manufacturing according to claim 1, wherein the preheating is performed before the forging.
12. The method according to claim 11, wherein the preheating temperature is 140 to 160 ℃.
13. The method according to claim 11, wherein the preheating time is 10-15 min.
14. The method according to claim 1, wherein the forged aluminum or aluminum alloy target blank has dimensions of (765-770 mm) x (188-192 mm) x (120-125 mm).
15. The method according to claim 1, wherein the temperature of the secondary heat treatment is 290 to 310 ℃.
16. The method according to claim 1, wherein the time of the secondary heat treatment is 25 to 40 min.
17. The method according to claim 1, wherein the temperature of the first pass of rolling is 295-305 ℃.
18. The method according to claim 1, wherein the rolling passes are 3.
19. The preparation method according to claim 1, wherein the reduction amount of the fourth pass of rolling is 5-10 mm.
20. The preparation method according to claim 1, wherein the reduction amount of the fifth pass of rolling is 5-10 mm.
21. The preparation method according to claim 1, wherein the total rolling reduction is 98-102 mm.
22. The production method according to claim 1, wherein the temperature after rolling is room temperature.
23. The method of claim 1, wherein the rolling is followed by flattening.
24. The method of claim 23, wherein the flattened bow is no greater than 1 mm.
25. The method according to claim 1, wherein the temperature of the third heat treatment is 245 to 255 ℃.
26. The method according to claim 1, wherein the time of the third heat treatment is 13 to 17 min.
27. The method of claim 1, comprising the steps of:
(1) cutting to obtain aluminum or aluminum alloy target blanks with the sizes of (290-295 mm) × (245-250 mm); preheating the obtained aluminum or aluminum alloy target blank at the temperature of 140-160 ℃ for 10-15 min, and then forging and stretching, wherein the size of the forged aluminum or aluminum alloy target blank is (198-202 mm) × (298-302 mm);
(2) carrying out primary heat treatment at 295-305 ℃ for 58-62 min;
(3) preheating for 10-15 min at the temperature of 140-160 ℃, and then forging, wherein the size of the forged aluminum or aluminum alloy target blank is 765-770 mm multiplied by 188-192 mm multiplied by 120-125 mm;
(4) carrying out secondary heat treatment at 290-310 ℃ for 25-40 min;
(5) rolling for 3-5 times, wherein the pressure drop of the first pass is 48-52 mm, the pressure drop of the second pass is 38-42 mm, the pressure drop of the third pass is 8-12 mm, the pressure drop of the fourth pass is 5-10 mm, the pressure drop of the fifth pass is 5-10 mm, and the total pressure drop is 98-102 mm; leveling after rolling, wherein the curvature after leveling is not more than 1 mm;
(6) and carrying out three times of heat treatment at 245-255 ℃ for 13-17 min to obtain the high-purity aluminum or aluminum alloy target material.
28. A high purity aluminum or aluminum alloy target material prepared by the preparation method according to any one of claims 1 to 27, wherein the purity of the high purity aluminum or aluminum alloy target material is 5N to 5N 5.
29. The high purity aluminum or aluminum alloy target material as claimed in claim 28, wherein the maximum grain size of the high purity aluminum or aluminum alloy target material is not more than 200 μm.
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| CN113897566B (en) * | 2021-09-27 | 2022-07-29 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity aluminum target |
| CN113857402A (en) * | 2021-09-27 | 2021-12-31 | 宁波江丰电子材料股份有限公司 | Preparation method of alloy high-purity copper target material |
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