CN116904942A - Aluminum-based alloy target and preparation method thereof - Google Patents
Aluminum-based alloy target and preparation method thereof Download PDFInfo
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- CN116904942A CN116904942A CN202310959111.4A CN202310959111A CN116904942A CN 116904942 A CN116904942 A CN 116904942A CN 202310959111 A CN202310959111 A CN 202310959111A CN 116904942 A CN116904942 A CN 116904942A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 74
- 239000000956 alloy Substances 0.000 title claims abstract description 74
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 41
- 239000002184 metal Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 28
- 238000001192 hot extrusion Methods 0.000 claims abstract description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000011049 filling Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 35
- 238000000137 annealing Methods 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 13
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000013077 target material Substances 0.000 abstract description 20
- 230000008569 process Effects 0.000 abstract description 9
- 230000000052 comparative effect Effects 0.000 description 24
- 239000000463 material Substances 0.000 description 19
- 238000001513 hot isostatic pressing Methods 0.000 description 17
- 238000007872 degassing Methods 0.000 description 16
- 238000011282 treatment Methods 0.000 description 14
- 239000011812 mixed powder Substances 0.000 description 12
- 238000012545 processing Methods 0.000 description 12
- 229910000599 Cr alloy Inorganic materials 0.000 description 8
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 description 8
- 239000000788 chromium alloy Substances 0.000 description 8
- 238000005098 hot rolling Methods 0.000 description 8
- 229910001069 Ti alloy Inorganic materials 0.000 description 7
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 238000003754 machining Methods 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 6
- 238000000576 coating method Methods 0.000 description 4
- 238000009694 cold isostatic pressing Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B22F3/10—Sintering only
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
Abstract
The application relates to the technical field of targets, and particularly discloses an aluminum-based alloy target and a preparation method thereof. The preparation method of the aluminum-based alloy target provided by the application comprises the following steps: firstly, filling metal powder into a die, carrying out vacuum degassing sintering at 400-520 ℃ to obtain a blank, and then directly carrying out hot extrusion molding on the blank to obtain an aluminum-based alloy target; the metal powder comprises more than 60at% of aluminum powder based on 100at% of the metal powder; the balance is one or more of chromium powder, titanium powder, silicon powder, tungsten powder, vanadium powder, boron powder, tantalum powder, yttrium powder, niobium powder, molybdenum powder and zirconium powder; the application also provides an aluminum-based alloy target material obtained by the method. The preparation method of the aluminum-based alloy target material provided by the application has the advantages of low equipment cost, short process flow, uniform metallographic structure, high density and excellent comprehensive mechanical property.
Description
Technical Field
The application relates to the technical field of targets, in particular to an aluminum-based alloy target and a preparation method thereof.
Background
PVD hard coating is a surface coating made of metal, alloy, etc. with good hardness, wear resistance, corrosion resistance and high temperature stability. The aluminum-based alloy target is a key consumable for preparing the high-performance PVD hard coating.
The traditional preparation process of the aluminum-based alloy target material is a hot isostatic pressing method, the method is to put metal mixed powder into a hot isostatic pressing die, and directly hot isostatic press the metal mixed powder into a compact target material after degassing, but the method has the defects of high equipment cost, high running cost and the like. In recent years, researchers have developed a new preparation process of an aluminum-based alloy target, wherein raw materials are densified into a blank by adopting cold isostatic pressing equipment, and then the blank is subjected to hot rolling treatment, so that the aluminum-based alloy target is obtained; the cold isostatic press used in this method is still relatively expensive and the hot rolling treatment process requires multi-pass rolling. Therefore, the method still has the defects of high production cost, complex process flow and the like, so that low-cost industrialized production is difficult to realize.
Disclosure of Invention
The application provides an aluminum-based alloy target and a preparation method thereof in order to further simplify the production process of the aluminum-based alloy target and reduce the production cost.
In a first aspect, the application provides a preparation method of an aluminum-based alloy target, which adopts the following technical scheme:
the preparation method of the aluminum-based alloy target comprises the following steps: firstly, filling metal powder into a die, carrying out vacuum degassing sintering at 400-520 ℃ to obtain a blank, and then directly carrying out hot extrusion molding on the blank to obtain an aluminum-based alloy target; the metal powder comprises more than 60at% of aluminum powder based on 100at% of the metal powder; the balance is one or more of chromium powder, titanium powder, silicon powder, tungsten powder, vanadium powder, boron powder, tantalum powder, yttrium powder, niobium powder, molybdenum powder and zirconium powder.
The application provides a preparation method of an aluminum-based alloy target, which comprises the steps of vacuum degassing and sintering metal powder, and then directly hot extrusion molding, so that plastic deformation and densification of the metal powder simultaneously occur in the hot extrusion process, and the aluminum-based alloy target is formed in one step. Compared with the process of carrying out hot rolling treatment after cold isostatic pressing in the related technology, the preparation method reduces the treatment process of cold isostatic pressing, greatly shortens the process flow and reduces the production cost; in addition, the hot rolling treatment in the related art is only suitable for the target material with small deformation, the hot extrusion forming treatment can be suitable for the target material with large deformation, and the aluminum-based alloy target material obtained through hot extrusion forming has smaller structure grain size, higher compactness and better comprehensive mechanical property.
In the present application, vacuum degassing sintering includes two roles of degassing and sintering: the degassing function is mainly to remove gas in the metal powder, so that on one hand, the resistance in extrusion molding is reduced, the metal powder is easier to densify, and on the other hand, the gas impurity content in the aluminum-based alloy target finished product is reduced; the sintering function is to make the metal powder reach a certain metallurgical bonding degree, so that the metal powder has a certain shaping deformation capacity, and is convenient for extrusion molding of subsequent densification. In addition, the vacuum degassing sintering process is carried out at 400-520 ℃, and extrusion molding is directly carried out without heating after the vacuum degassing sintering is finished. In the related art, after the vacuum degassing sintering is completed, the jacket is cooled to room temperature, and then is reheated for hot isostatic pressing or hot rolling. Therefore, the preparation process of the aluminum-based alloy target material provided by the application has the advantages of simple operation steps, low energy consumption, low production cost and the like.
According to the application, through experimental research, when the aluminum powder content in the metal powder is less than or equal to 50at%, the plasticity of the blank is lower, and the blank cannot be extruded and formed, so that cracking is caused. When the vacuum degassing sintering temperature is less than 400 ℃, on one hand, the degassing is not thorough enough, and the residual gas in the blank can reduce the density of the final target; on the other hand, the degassing sintering temperature is low, the molding deformation capability of the material is poor, and extrusion cracking is caused; when the vacuum degassing sintering temperature is higher than 520 ℃, the metal powder can react, so that the plasticity of the blank is lower, the blank cannot be extruded and formed, and the blank is cracked. Therefore, the aluminum powder content and the vacuum degassing sintering temperature in the metal powder are controlled within the ranges, so that extrusion molding of a blank can be realized, and the obtained aluminum-based alloy target material has uniform metallographic structure, high compactness and excellent comprehensive mechanical property.
Preferably, the hot extrusion molding is performed at a pressure of 100-2000T and a temperature of 400-520 ℃.
In the application, the extruded blank is required to be sprayed with water to be rapidly cooled, so that the aluminum-based alloy target material is endowed with excellent mechanical properties.
In the application, the raw materials for preparing the aluminum-based alloy target are all metal powder, and the reaction between the metal powder can be effectively avoided by controlling the vacuum degassing sintering temperature and the extrusion temperature within the ranges.
In some embodiments, the metal powder is aluminum powder and chromium powder, and the vacuum degassing sintering temperature and the extrusion forming temperature are controlled to be 400-520 ℃, preferably 400-470 ℃, and further preferably 400 ℃ or 450 ℃; the aluminum powder content may be 60at%, 70at% or 90at%, and the chromium powder content may be 10at%, 30at% or 40at%.
In some embodiments, the metal powder is aluminum powder and titanium powder, and the vacuum degassing sintering temperature and the extrusion forming temperature should be controlled to be 400-520 ℃, preferably 400-500 ℃, and further preferably 400 ℃, 450 ℃ or 500 ℃; the aluminum powder content may be 60at%, 65at% or 67at%, and the titanium powder content may be 33at%, 35at% or 40at%.
Preferably, the vacuum degree of the vacuum degassing sintering is less than or equal to 2 multiplied by 10 -3 Pa, and vacuum heat preservation time is more than or equal to 4 hours.
Preferably, the heat treatment temperature of the annealing heat treatment step is 200-400 ℃, and the heat treatment heat preservation time is 2-5h.
According to the application, the annealing heat treatment is carried out on the extruded blank, so that the internal structure and grain size of the target can be effectively controlled, and the internal stress of the target is eliminated, thereby being beneficial to the subsequent mechanical processing of the target. When the annealing temperature is too high or the annealing time is too long, the Al of the target matrix reacts with the alloy elements to generate intermetallic compounds, and the different alloy elements react with the Al at different temperatures, so that once the alloying reaction occurs, the metallographic structure and strength of the aluminum-based alloy target can be deteriorated, and even the subsequent coating process is influenced; when the annealing temperature is too low or the annealing time is too short, a large amount of internal stress formed in the extrusion processing process cannot be completely eliminated, so that the toughness and the processing performance of the aluminum-based alloy target material can be affected. Therefore, the application further controls the annealing heat treatment temperature and time within the above range, and the obtained aluminum-based alloy target material has uniform metallographic structure, high compactness and excellent comprehensive mechanical property.
In some specific embodiments, the annealing heat treatment step may have a heat treatment temperature of 200 ℃, 300 ℃, 350 ℃, or 400 ℃.
In some specific embodiments, the annealing heat treatment step may have a heat treatment soak time of 2 hours, 3 hours, 4 hours, or 5 hours.
Preferably, the extrusion speed is 10-20m/min, and the extrusion ratio is (3-5): 1, the extrusion die angle is 45-60 degrees.
Preferably, the particle size of the metal powder is 20-100 μm.
In a specific embodiment, the metal powder has a particle size of 30-50 μm.
In the application, the aluminum-based alloy target is prepared by removing the sheath from the heat-treated blank, machining, cleaning and packaging.
In a second aspect, the present application provides an aluminum-based alloy target prepared by the aforementioned method for preparing an aluminum-based alloy target.
Preferably, the compactness of the aluminum-based alloy target is more than or equal to 99.3 percent, and the average grain size of the aluminum matrix is less than or equal to 10 mu m.
In the application, aluminum-based alloy targets with different types or sizes can be obtained by changing the shape and the size of the extrusion die of the extruder, and the shape of the aluminum-based alloy targets can be plates or bars.
In a specific embodiment, the aluminum-based alloy target is a sheet material, and the dimensions of the aluminum-based alloy target are 740mm in length by 170mm in width by 20mm in thickness. In summary, the application has the following beneficial effects:
1. compared with the related technology, the preparation method of the aluminum-based alloy target material omits the use of hot isostatic pressing equipment and cold isostatic pressing equipment, simplifies the process steps and greatly reduces the production cost of the aluminum-based alloy target material.
2. The aluminum-based alloy target prepared by the preparation method provided by the application has the advantages of small grain size, uniform metallographic structure, high compactness and excellent comprehensive mechanical property.
Drawings
Fig. 1 is a diagram showing a microstructure of x 100 times of an aluminum chrome alloy target provided in example 2 of the present application.
Fig. 2 is a 100-fold metallographic microstructure of the aluminum-titanium alloy target provided in example 5 of the present application.
Fig. 3 is a diagram showing a metallographic microstructure of x 100 times that of the aluminum chrome alloy target provided in comparative example 5 of the present application.
Fig. 4 is a 100 x metallographic microstructure of the aluminum-titanium alloy target provided in comparative example 6 of the present application.
FIG. 5 is a drawing of a billet after extrusion of aluminum chrome alloy according to example 2 of the present application.
FIG. 6 is a drawing of a billet after extrusion of the aluminum-titanium alloy of example 5 of the present application.
FIG. 7 is a drawing of a billet after extrusion of the aluminum chrome alloy of comparative example 1 of the application.
FIG. 8 is a drawing of a preform after extrusion of an aluminum-titanium alloy according to comparative example 2 of the present application.
Detailed Description
The application provides a preparation method of an aluminum-based alloy target, which comprises the following steps:
(1) Preparing raw materials: and mixing the metal powder in a mixer to obtain mixed powder. The metal powder comprises more than 60at% of aluminum powder, and the balance of one or more of chromium powder, titanium powder, silicon powder, tungsten powder, vanadium powder, boron powder, tantalum powder, yttrium powder, niobium powder, molybdenum powder and zirconium powder.
(2) Vacuum degassing and sintering: filling the mixed powder into a sheath die for degassing treatment; the sintering temperature of vacuum degassing is 400-520 ℃, and the vacuum degree in the die after degassing is less than or equal to 2 multiplied by 10 -3 Pa, and the heat preservation time of the vacuum degree is more than or equal to 4 hours.
(3) Extrusion molding: directly feeding the degassed material blank out of the furnace into an extruder for extrusion molding, preheating an extrusion die before extrusion, wherein the heating temperature is 400-520 ℃, the hot extrusion pressure is 100-2000T, the extrusion speed is 10-20m/min, the extrusion ratio (3-5) is 1, the extrusion die angle is 45-60 degrees, and the extruded material blank is rapidly cooled by water spraying.
(4) Annealing heat treatment: and carrying out annealing heat treatment on the cooled blank, wherein the heat treatment temperature is 200-400 ℃, and the heat treatment heat preservation time is 2-5h. Further, the heat treatment temperature is 250-350 ℃, and the heat treatment heat preservation time is 3-5h.
(5) And (3) processing a finished product: the heat-treated blank is subjected to sheath removal, machining, cleaning and packaging to obtain the aluminum-based alloy target.
The metal powder used in the present application has a particle size of 30 to 50. Mu.m, and is commercially available.
The present application will be described in further detail with reference to examples, performance test and accompanying drawings.
Examples 1 to 10
Examples 1-10 respectively provide a method for preparing an aluminum-based alloy target, which is different in that: the metal powder and the vacuum degassing sintering temperature are shown in table 1.
The preparation method of the aluminum chromium alloy target comprises the following steps:
(1) Metal powders (as shown in table 1) were mixed in a mixer to obtain mixed powders.
(2) Vacuum degassing and sintering: filling the mixed powder into a sheath die for degassing treatment;the sintering temperature of vacuum degassing is 400-520 ℃, and the vacuum degree in the die is 1 multiplied by 10 after degassing -3 Pa, the incubation time of the above vacuum degree is 4 hours.
(3) Extrusion molding: directly feeding the degassed material blank out of the furnace into an extruder for extrusion molding, preheating an extrusion die before extrusion, wherein the heating temperature is 450 ℃, the hot extrusion pressure is 500T, the extrusion speed is 15m/min, the extrusion ratio is 4:1, the extrusion die angle is 50 degrees, and the extruded material blank is rapidly cooled by water spraying.
(4) Annealing heat treatment: and carrying out annealing heat treatment on the cooled blank, wherein the heat treatment temperature is 350 ℃, and the heat treatment heat preservation time is 3 hours.
(5) And (3) processing a finished product: the heat-treated blank is subjected to sheath removal, machining, cleaning and packaging to obtain the aluminum-based alloy target material with the length of 740mm, the width of 170mm and the thickness of 20 mm.
TABLE 1 Metal powders and vacuum degassing sintering temperatures in examples 1-10
Examples 11 to 13
Examples 11-13 were conducted in accordance with the method of example 5 except that: the heat treatment temperature in the annealing heat treatment step is specifically shown in table 2.
TABLE 2 heat treatment temperatures for the annealing heat treatment steps in example 5, examples 11-13
| Examples | Heat treatment temperature (. Degree. C.) |
| 5 | 350 |
| 11 | 200 |
| 12 | 300 |
| 13 | 400 |
Examples 14 to 16
Examples 14-16 were conducted in accordance with the method of example 5 except that: the holding time of the annealing heat treatment step is shown in Table 3.
TABLE 3 incubation time for annealing heat treatment steps in example 5, examples 14-16
| Examples | Time of thermal insulation (h) |
| 5 | 3 |
| 14 | 2 |
| 15 | 4 |
| 16 | 5 |
Comparative example 1
Comparative example 1 provides a method for preparing an aluminum chromium alloy target, which is different from example 2 in that: the metal powder comprises the following components: cr50at% and Al50at%.
Comparative example 2
Comparative example 2 provides a method for preparing an aluminum titanium alloy target, which is different from example 5 in that: the metal powder comprises the following components: 50at% of Ti and 50at% of Al.
Comparative example 3
Comparative example 3 provides a method for preparing an aluminum chromium alloy target, which is different from example 2 in that: the vacuum degassing sintering temperature was 550 ℃.
Comparative example 4
Comparative example 4 provides a method of preparing an aluminum chromium alloy target, which differs from example 5 in that: the vacuum degassing sintering temperature was 550 ℃.
Comparative example 5
Comparative example 5 provides a method of preparing an aluminum chromium alloy target,
(1) The metal powder (Cr 30at% and Al70 at%) was mixed in a mixer to obtain a mixed powder.
(2) Vacuum degassing and sintering: filling the mixed powder into a sheath die for degassing treatment; the degassing temperature was 400℃and the degree of vacuum in the die after degassing was 1X 10 -3 Pa, the vacuum degree heat preservation time is 4h.
(3) And (3) hot isostatic pressing sintering: and (3) carrying out hot isostatic pressing treatment on the degassed and discharged blank, wherein the hot isostatic pressing sintering temperature is 450 ℃, the hot isostatic pressing pressure is 130Mpa, and the hot isostatic pressing sintering time is 2h.
(4) And (3) processing a finished product: and removing the sheath of the blank after the hot isostatic pressing treatment, machining, cleaning and packaging to obtain the aluminum-chromium alloy target.
Comparative example 6
Comparative example 6 provides a method for preparing an aluminum-titanium alloy target, comprising the following steps:
(1) The metal powder (Ti 33at% and Al67 at%) was mixed in a mixer to obtain a mixed powder.
(2) Vacuum degassing and sintering: filling the mixed powder into a sheath mold for degassing at 500 deg.C, and vacuum degree in the mold of 1×10 -3 Pa, the vacuum degree heat preservation time is 4h.
(3) And (3) hot isostatic pressing sintering: and (3) carrying out hot isostatic pressing treatment on the degassed and discharged blank, wherein the hot isostatic pressing sintering temperature is 450 ℃, the hot isostatic pressing pressure is 130Mpa, and the hot isostatic pressing sintering time is 2h.
(4) And (3) processing a finished product: and removing the sheath of the blank after the hot isostatic pressing treatment, machining, cleaning and packaging to obtain the aluminum-titanium alloy target.
Comparative example 7
The preparation method of the aluminum chromium alloy target comprises the following steps:
(1) The metal powder (Cr 30at% and Al70 at%) was mixed in a mixer to obtain a mixed powder.
(2) Cold press molding: the mixed powder was charged into a 150mm×150mm×50mm cold press die (the cold press die is die steel, the die roughness is ra0.1, the die hardness is 90 HRA), held at a cold press pressure of 130MPa for 10s, and pressed into a cold pressed compact with a density of 75%, the height of the pressed compact being 50mm.
(3) Vacuum degassing and sintering: filling the cold-pressed blank into a mould for degassing treatment; the degassing temperature was 400℃and the degree of vacuum in the die after degassing was 1X 10 -3 Pa, the vacuum degree heat preservation time is 4h.
(4) And (3) hot rolling: and hot rolling the degassed blank, wherein the initial rolling temperature is 500 ℃, the final rolling temperature is 350 ℃, the rolling reduction is 60%, the rolling passes are 3 times, and the rolling speed is 0.8m/s.
(5) Annealing heat treatment: annealing heat treatment is carried out on the rolled blank, the heat treatment temperature is 350 ℃, and the heat treatment heat preservation time is 3 hours;
(6) And (3) processing a finished product: the heat-treated blank is subjected to sheath removal, machining, cleaning and packaging to obtain the aluminum chromium alloy target.
Performance test
The properties of the aluminum-based alloy targets obtained in examples 1 to 16 and comparative examples 1 to 7 were examined, and the results are shown in Table 4.
1. The method for detecting the average grain size of the aluminum matrix comprises the following steps: reference is made to GB/T6394-2017 method for determination of average grain size of metals.
2. The density detection method comprises the following steps: reference is made to GB/T3850-2015 methods for determining density of dense sintered Metal Material and cemented carbide.
3. The detection method of tensile strength, yield strength and elongation comprises the following steps: reference is made to GB/T228.1-2021 section 1, metal tensile test: room temperature test methods.
TABLE 4 Performance test results of aluminum-based alloy targets obtained in examples 1 to 16 and comparative examples 1 to 7
According to the detection results of examples 1-16, the preparation method of the aluminum-based alloy target material provided by the application can prepare the aluminum-based alloy target material with the grain size smaller than 11 mu m and the compactness of 99.0%.
In comparative examples 1 to 2, since the alloy element content was too high and the atomic ratio reached 50at%, the plastic deformation ability of the material was drastically lowered, resulting in cracking during extrusion processing and failure of extrusion processing, as shown in fig. 7 to 8.
In comparative examples 3 to 4, the alloy element and the matrix Al react vigorously due to the excessively high heating temperature, so that a hard and brittle intermetallic compound phase is generated, and the material is shaped and disappears, so that the extrusion deformability is lost, the extrusion is cracked, and the processing production cannot be performed.
The preparation process of the hot isostatic pressing is adopted in the comparative examples 5-6, the production process has higher production equipment cost, the obtained aluminum-based alloy target material has coarse grain structure, the average grain size is as high as 35 mu m, the mechanical comprehensive performance of the material is slightly poor, and the metallographic microstructure of the aluminum-based alloy target material obtained in the comparative examples 5-6 is shown in the figures 3-4.
Comparative example 7 adopts a hot rolling preparation process, and the obtained aluminum-based alloy target material has excellent grain structure, compactness and comprehensive mechanical properties, but the production process is complex in flow, complex in operation and high in equipment cost, so that the preparation process is not suitable for industrial production.
As can be seen from the test results of examples 1-3 and examples 5-7, as the content of the alloy element increases, the tensile strength and yield strength of the extruded material increase due to the particle strengthening effect, but the performance of the extruded material decreases after the content of the alloy element increases to a certain amount, mainly because the plastic deformation capability of the material decreases due to the increase of the alloy element content, and the extrusion processing density decreases; the increase in alloying elements correspondingly reduces the toughness of the material and therefore its elongation becomes lower.
The test results of examples 3 to 4, 5 and 8 to 10 show that the material has better molding deformation capability and slightly improved compactness with the increase of the extrusion temperature, so that the mechanical properties are slightly increased.
As is clear from the results of the examination of examples 5 and examples 11 to 13, the toughness of the material became better with an increase in the annealing temperature, and therefore the yield strength and elongation thereof increased, and the tensile strength of the material was slightly lowered due to the disappearance of the compression stress.
The test results of examples 5 and examples 14 to 16 show that as the annealing heat-preservation time is prolonged, the extrusion internal stress of the material disappears more, the toughness of the material is better and the elongation is larger, but after a certain heat-preservation time, the reaction starts to occur in the material, the toughness is poor, and therefore the elongation and the yield strength are reduced, and the tensile strength is increased.
While the application has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the application and are intended to be within the scope of the application as claimed.
Claims (9)
1. The preparation method of the aluminum-based alloy target is characterized by comprising the following steps of:
firstly, filling metal powder into a die, carrying out vacuum degassing sintering at 400-520 ℃ to obtain a blank, and then directly carrying out hot extrusion molding on the blank to obtain an aluminum-based alloy target; the metal powder contains 60at% or more of aluminum powder based on 100at% of the metal powder; the balance is one or more of chromium powder, titanium powder, silicon powder, tungsten powder, vanadium powder, boron powder, tantalum powder, yttrium powder, niobium powder, molybdenum powder and zirconium powder.
2. The method for producing an aluminum-based alloy target according to claim 1, wherein the hot extrusion is performed at a pressure of 100 to 2000T and a temperature of 400 to 520 ℃.
3. The method of producing an aluminum-based alloy target according to claim 1, wherein the vacuum degassing sintering temperature is 400-470 ℃.
4. The method for producing an aluminum-based alloy target according to claim 1, wherein the vacuum degree of vacuum degassing sintering is 2×10 or less -3 Pa, and vacuum heat preservation time is more than or equal to 4 hours.
5. The method for preparing an aluminum-based alloy target according to claim 1, wherein the extruded preform is further subjected to an annealing heat treatment at 200-400 ℃ for 2-5 hours.
6. The method for producing an aluminum-based alloy target according to claim 1, wherein the extrusion speed is 10-20m/min, and the extrusion ratio is (3-5): 1, the extrusion die angle is 45-60 degrees.
7. The method for producing an aluminum-based alloy target according to claim 1, wherein the particle size of the metal powder is 20 to 100 μm.
8. An aluminum-based alloy target produced by the production method of an aluminum-based alloy target according to any one of claims 1 to 7.
9. The aluminum-based alloy target according to claim 8, wherein the density of the aluminum-based alloy target is more than or equal to 99.0%, and the average grain size of an aluminum matrix is less than or equal to 10 μm.
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