CN112048703A - Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof - Google Patents
Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof Download PDFInfo
- Publication number
- CN112048703A CN112048703A CN202010710119.3A CN202010710119A CN112048703A CN 112048703 A CN112048703 A CN 112048703A CN 202010710119 A CN202010710119 A CN 202010710119A CN 112048703 A CN112048703 A CN 112048703A
- Authority
- CN
- China
- Prior art keywords
- aluminum
- sputtering target
- neodymium alloy
- alloy rotary
- neodymium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005477 sputtering target Methods 0.000 title claims abstract description 79
- 229910000583 Nd alloy Inorganic materials 0.000 title claims abstract description 74
- UBSJOWMHLJZVDJ-UHFFFAOYSA-N aluminum neodymium Chemical compound [Al].[Nd] UBSJOWMHLJZVDJ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000013077 target material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004544 sputter deposition Methods 0.000 claims abstract description 59
- 238000001125 extrusion Methods 0.000 claims description 41
- 238000005266 casting Methods 0.000 claims description 28
- 238000003754 machining Methods 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 23
- 229910052779 Neodymium Inorganic materials 0.000 claims description 18
- 238000003723 Smelting Methods 0.000 claims description 18
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 17
- 238000012545 processing Methods 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000005204 segregation Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 18
- 238000003466 welding Methods 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- -1 argon ions Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 1
- DJPURDPSZFLWGC-UHFFFAOYSA-N alumanylidyneborane Chemical compound [Al]#B DJPURDPSZFLWGC-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- 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
-
- 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
-
- 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
-
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to an aluminum-neodymium alloy rotary sputtering target material and a preparation method thereof. The aluminum-neodymium alloy rotary sputtering target comprises a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends which are respectively positioned on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed. In the aluminum-neodymium alloy rotary sputtering target, on one hand, the sputtering end and the mounting end are integrally formed, so that the sputtering effect can be prevented from being influenced by poor welding quality; on the other hand, the outermost layer of the body is an oxide layer, so that the body is guaranteed to have enough hardness and is not easy to damage. The whole enables the aluminum-neodymium alloy rotary sputtering target material to be beneficial to application.
Description
Technical Field
The invention relates to the technical field of rotary sputtering targets, in particular to an aluminum-neodymium alloy rotary sputtering target and a preparation method thereof.
Background
The vacuum coating is a process of placing a material to be coated and a substrate to be coated in a vacuum chamber, heating the material to be coated by adopting a certain method to evaporate or sublimate the material, and sputtering the material to be coated on the surface of the substrate to be coated for condensation and film formation. The conventional vacuum coating technology is magnetron sputtering coating, which is a coating technology that a coating material is used as a target cathode, argon ions are used for bombarding a target material to generate cathode sputtering, and target material atoms are sputtered onto a workpiece to form a deposition layer.
Compared with the rotary tube target, the planar target has lower material utilization rate and shorter service life, so that the target material product is gradually upgraded from the planar target to the rotary tube target. The rotating tube target has higher requirements on processing precision and production process, and has requirements on material density, purity, grain size, uniformity, dimensional precision and the like.
The aluminum neodymium rotating tube target material is mainly used in the flat panel display industry. The two ends of the traditional aluminum neodymium rotating tube target are welded, and the poor welding quality easily causes air leakage and water leakage, so that the effect of sputtering equipment is greatly influenced, and the application is not facilitated.
Disclosure of Invention
Therefore, it is necessary to provide an aluminum-neodymium alloy rotary sputtering target and a preparation method thereof, which can avoid the adverse effect of the welding quality on the sputtering effect and can not be easily damaged, aiming at the problem of how to avoid the adverse effect of the welding quality on the sputtering effect of the aluminum-neodymium alloy rotary sputtering target and can not be easily damaged.
The rotary aluminum-neodymium alloy sputtering target comprises a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends which are respectively positioned on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed.
In the aluminum-neodymium alloy rotary sputtering target, on one hand, the sputtering end and the mounting end are integrally formed, so that the sputtering effect can be prevented from being influenced by poor welding quality; on the other hand, the outermost layer of the body is an oxide layer, so that the body is guaranteed to have enough hardness and is not easy to damage. The whole enables the aluminum-neodymium alloy rotary sputtering target material to be beneficial to application.
In one embodiment, the thickness of the oxide layer is 20 μm to 35 μm.
A preparation method of an aluminum-neodymium alloy rotary sputtering target comprises the following steps:
uniformly mixing 95-99.9% of aluminum and 0.1-5% of neodymium according to atomic percentage, smelting, and then sequentially casting, molding, extruding and annealing to obtain a precursor;
carrying out surface hard oxidation treatment on the precursor to form an oxide layer on the surface of the precursor, and then carrying out machining treatment to obtain an aluminum-neodymium alloy rotary sputtering target; the rotary aluminum-neodymium alloy sputtering target comprises a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends which are respectively positioned on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed.
By adopting the preparation method of the aluminum-neodymium alloy rotary sputtering target material, the integrated aluminum-neodymium alloy rotary sputtering target material can be prepared, the sputtering effect can be prevented from being influenced by poor welding quality during use, and the body is ensured to have enough hardness, so that the body is not easy to damage. The whole enables the aluminum-neodymium alloy rotary sputtering target material to be beneficial to application.
In one embodiment, the step of mixing aluminum and neodymium comprises: firstly adding aluminum ingot and then adding neodymium block.
In one embodiment, the smelting conditions are as follows: smelting at 1100-1200 deg.c for 20-60 min, skimming slag, mixing with refiner and stilling to obtain mixed metal liquid.
In one embodiment, the step of casting is as follows: semi-continuously casting the smelted mixed molten metal to obtain a casting rod with a preset size; in the casting process, the casting temperature is 685-715 ℃ and the casting speed is 80-100 mm/min.
In one embodiment, after the casting and forming and before the extrusion processing, the method further comprises the step of performing first machining processing on the cast rod after the casting and forming;
the first machining processing step comprises the following steps: and cutting off the segregation areas at the head and the tail of the cast rod and oxide skins on the outer surfaces of the segregation areas so as to reach the preset size before extrusion.
In one embodiment, the extrusion process comprises the steps of: heating the cast rod after the first machining to 320-380 ℃, heating the die and the extrusion needle to 350-450 ℃, cleaning the inner cylinder of the die before extrusion, and then maintaining the extrusion speed at 0.5-1.0 m/min until extrusion to obtain an extrusion blank with a preset size.
In one embodiment, the annealing process comprises the following steps: and (3) preserving the temperature of the extrusion blank within the temperature range of 250-400 ℃ for 2-5 h, and then cooling to obtain the extrusion blank after annealing treatment.
In one embodiment, after the annealing treatment and before the surface hard oxidation treatment, the method further comprises the step of performing secondary machining treatment on the annealed extrusion blank;
the second machining processing step comprises the following steps: and processing the two ends of the annealed extrusion blank to the size of a finished product, and processing the sputtering area of the annealed extrusion blank to leave a preset allowance to obtain a precursor.
In one embodiment, the surface hard oxidation treatment comprises the following steps: and treating the surface of the precursor by using acid liquor, and performing hole sealing treatment to form an oxide layer on the surface of the precursor.
In one embodiment, the acid solution is a sulfuric acid solution or an oxalic acid solution; the acid liquor has a mass percentage concentration of 10-30%.
Drawings
FIG. 1 is a schematic view of an aluminum-neodymium alloy rotary sputtering target according to an embodiment of the present invention;
FIG. 2 is a schematic cross-sectional view of an Al-Nd alloy rotating sputtering target along a central plane according to one embodiment of the present invention;
FIG. 3 is an as-cast phase diagram of the aluminum-neodymium alloy rotary sputtering target of example 4;
FIG. 4 is an as-annealed gold phase diagram of the aluminum-neodymium alloy rotary sputtering target of example 4.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The aluminum-neodymium alloy rotary sputtering target of the present invention may contain impurities in a stoichiometric range.
Referring to fig. 1 and 2, an aluminum-neodymium alloy rotary sputtering target 100 according to an embodiment of the present invention includes a body 110, an outermost layer of the body 110 is an oxide layer 112, the body 110 includes a sputtering end 114 and a mounting end 116 respectively located at two sides of the sputtering end 114, and the sputtering end 114 and the mounting end 116 are integrally formed. The oxide layer 112 is formed by surface hard oxidation treatment, so that the body 110 has certain hardness and is not easy to damage in the using process. The sputtering tip 114 is used to provide a sputtering area during magnetron sputtering. Wherein the mounting end 116 is configured to be mounted to a base of a sputtering apparatus.
In one embodiment, the oxide layer 112 has a thickness of 20 μm to 35 μm. Therefore, the hardness can be improved to a certain degree, and the sputtering effect can be prevented from being influenced by too high thickness of the oxide layer.
In the aluminum-neodymium alloy rotary sputtering target, on one hand, the sputtering end and the mounting end are integrally formed, so that the sputtering effect can be prevented from being influenced by poor welding quality; on the other hand, the outermost layer of the body is an oxide layer, so that the body is guaranteed to have enough hardness and is not easy to damage. The whole enables the aluminum-neodymium alloy rotary sputtering target material to be beneficial to application.
The preparation method of the aluminum-neodymium alloy rotary sputtering target material comprises the following steps:
s10, mixing 95-99.9% of aluminum and 0.1-5% of neodymium uniformly according to atomic percentage, smelting, and then sequentially casting, molding, extruding and annealing to obtain the precursor.
Wherein, the atomic percentage of the aluminum to the neodymium is (95-99.9): (0.1-5). The rotary sputtering target material obtained by adopting the aluminum-neodymium alloy with the atomic percentage has better performance.
The integrated aluminum-neodymium alloy rotary sputtering target can be obtained by adopting the preparation method.
In one embodiment, the step of mixing aluminum and neodymium comprises: firstly adding aluminum ingot and then adding neodymium block. This can reduce the smelting loss of neodymium.
In one embodiment, the smelting conditions are as follows: smelting at 1100-1200 deg.c for 20-60 min, skimming slag, mixing with refiner and stilling to obtain mixed metal liquid. Among them, the refiner is preferably an aluminum-titanium-boron wire, an aluminum-titanium wire and an aluminum-boron wire.
In one preferred embodiment, the steps of homogenizing and melting aluminum and neodymium are as follows: the smelting temperature is maintained at 1100-1200 ℃, the aluminum ingot is smelted for 10-20 min, and then the neodymium block is added for smelting for 10-40 min.
It should be noted that, in the process of mixing and smelting aluminum and neodymium, the sequence of adding aluminum and neodymium is not limited. Or adding neodymium blocks, smelting for a period of time, and then adding aluminum ingots for smelting. Or simultaneously adding aluminum and neodymium to carry out smelting.
In one embodiment, the step of casting is as follows: semi-continuously casting the smelted mixed molten metal to obtain a casting rod with a preset size; in the casting process, the casting temperature is 685-715 ℃ and the casting speed is 80-100 mm/min.
In one embodiment, after the casting and forming and before the extrusion processing, the method further comprises the step of performing first machining processing on the cast rod after the casting and forming;
the first machining treatment comprises the following steps: and cutting off segregation areas at the head and the tail of the cast rod and oxide skins on the outer surfaces of the segregation areas so as to reach a preset size before extrusion.
In one embodiment, the extrusion process comprises the steps of: heating the cast rod after the first machining to 320-380 ℃, heating the die and the extrusion needle to 350-450 ℃, cleaning the inner cylinder of the die before extrusion, and then maintaining the extrusion speed at 0.5-1.0 m/min until extrusion to obtain an extrusion blank with a preset size.
In one embodiment, the annealing step comprises: and (3) preserving the temperature of the extrusion blank within the temperature range of 250-400 ℃ for 2-5 h, and then cooling to obtain the extrusion blank after annealing treatment. S20, carrying out surface hard oxidation treatment on the precursor to form an oxide layer on the surface of the precursor, and then carrying out machining treatment to obtain the aluminum-neodymium alloy rotary sputtering target; the aluminum-neodymium alloy rotary sputtering target comprises a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends which are respectively positioned on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed.
In one embodiment, after the annealing treatment and before the surface hard oxidation treatment, the method further comprises the step of performing secondary machining treatment on the annealed extrusion blank;
the second machining treatment comprises the following steps: and processing the two ends of the annealed extrusion blank to the size of a finished product, and processing the sputtering area of the annealed extrusion blank to leave a preset allowance to obtain a precursor.
In one embodiment, the surface hard oxidation treatment comprises the following steps: the surface of the precursor is treated with an acid solution, and then a sealing treatment is performed to form an oxide layer on the surface of the precursor.
In one embodiment, the acid solution is a sulfuric acid solution or an oxalic acid solution; the mass percentage concentration of the acid liquor is 10-30%. Thus, the rupture membrane can be prevented from cracking while the good coating effect is ensured.
In one embodiment, the oxide layer has a thickness of 20 μm to 35 μm. Therefore, the hardness can be improved to a certain degree, and the sputtering effect can be prevented from being influenced by too high thickness of the oxide layer.
Carrying out third machining treatment after the surface hard oxidation treatment, wherein the third machining treatment comprises the following steps: and processing the sputtering end into the size used by the client.
By adopting the preparation method of the aluminum-neodymium alloy rotary sputtering target material, the integrated aluminum-neodymium alloy rotary sputtering target material can be prepared, the sputtering effect can be prevented from being influenced by poor welding quality during use, and the body is ensured to have enough hardness, so that the body is not easy to damage. The whole enables the aluminum-neodymium alloy rotary sputtering target material to be beneficial to application.
The aluminum-neodymium alloy rotary sputtering target and the method for producing the same according to the present invention will be further described with reference to specific examples (the following examples, unless otherwise specified, do not contain other components not specifically indicated except for unavoidable impurities).
Examples 1 to 7
Weighing the raw materials according to the atomic percentage and table 1, adding an aluminum ingot and a neodymium block, maintaining the smelting temperature and the smelting time, and sequentially carrying out casting molding, first machining, extrusion, annealing, second machining, surface hard oxidation and third machining according to the casting molding conditions, the extrusion conditions, the annealing conditions and the surface hard oxidation conditions of the table 1 to obtain the aluminum-neodymium alloy rotary sputtering target material, wherein the thickness of an oxide layer in the aluminum-neodymium alloy rotary sputtering target material is shown in the table 1. The rotary aluminum-neodymium alloy sputtering target comprises a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends respectively located on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed.
Table 1 parameters in the steps of preparing aluminum-neodymium alloy rotary sputtering targets of examples 1 to 7
Comparative example 1
The aluminum-neodymium alloy rotary sputtering target of comparative example 1 differs from the aluminum-neodymium alloy rotary sputtering target of example 1 in that: the aluminum-neodymium alloy rotary sputtering target comprises a sputtering end and mounting ends respectively located on two sides of the sputtering end, wherein oxide layers are not arranged on the surfaces of the sputtering end and the mounting ends, the sputtering end and the mounting ends are made of different materials, and the sputtering end and the mounting ends are formed by welding.
And (3) testing:
1. and (3) component analysis:
glow discharge mass spectrometry (glow discharge mass spectrometry) was performed on the aluminum-neodymium alloy rotary sputtering target material of example 4, and table 2 was obtained.
Table 2 chemical composition and impurity content of the aluminum-neodymium alloy rotary sputtering target of example 4
As can be seen from table 2, the main chemical components of the aluminum-neodymium alloy rotary sputtering target of example 4 are: nd: 3.06 percent; purity of Al + Nd: 99.98 percent.
2. The as-cast and as-annealed grains of the alnd alloy rotary sputtering target of example 4 were tested to obtain fig. 3 and 4. As can be seen from FIGS. 3 and 4, the rotary sputtering target of the Al-Nd alloy according to example 4 had an as-cast average grain size of about 100 μm or more and an as-annealed average grain size of about 80 μm or less and about 20 μm or more.
3. The alnd alloy rotary sputtering targets of example 4 and comparative example 1 were tested for vickers hardness, and the test results were: the vickers hardness of the sputtering end of the aluminum-neodymium alloy rotary sputtering target of example 4 was 35, and the vickers hardness of the mounting end was 285; the alnd alloy rotary sputtering target of comparative example 1 had a vickers hardness of 30 at the sputtering end and 92 at the mounting end. As can be seen from the above tests, the vickers hardness of the mounting end of the aluminum-neodymium alloy rotary sputtering target of example 4 is much greater than that of the aluminum-neodymium alloy rotary sputtering target of comparative example 1.
4. The surface roughness of the sputtering surface of the aluminum-neodymium alloy rotary sputtering target of example 4 was measured, and the measurement results were: the arithmetic average roughness Ra is 1.0 μm or less, and the maximum height Rz is 6.3 μm or less.
5. The aluminum-neodymium alloy rotary sputtering targets of examples 1 to 7 and comparative example 1 were tested for crystal grain, density, and oxygen content, and table 3 was obtained.
The testing process of the crystal grains is as follows: taking a square block with the size of 10mm x 10mm on a finished target product, grinding and polishing the square block on a metallographic grinder, using sand paper with the sequence of 180-240-400-600-800-1200 meshes-deer skin polishing cloth, corroding the polished mirror surface by using a mixed acid solution after the surface of the metallographic block is like the mirror surface, washing the mirror surface under flowing distilled water after keeping for 10-30s, and observing the grain size of the mirror surface under a metallographic microscope after wiping by using alcohol.
The density test procedure was: a sample was taken from the target and the relative density was determined using Archimedes drainage.
The oxygen content was tested as follows: oxygen content determination was performed using an oxygen-nitrogen analyzer.
Table 3 test data for the aluminum-neodymium alloy rotary sputtering targets of examples 1-7 and comparative example 1
As can be seen from the data in table 3:
(1) compared with the sputtering target material of the comparative example 1, the aluminum-neodymium alloy rotary sputtering target materials of the embodiments 1 to 7 of the invention have larger reflectivity, which indirectly shows that the aluminum-neodymium alloy rotary sputtering target material of the invention can effectively improve the sputtering effect.
(2) Compared with the aluminum-neodymium alloy rotary sputtering target material of the comparative example 1, the aluminum-neodymium alloy rotary sputtering target materials of the embodiments 1 to 7 have longer oxidation resistance time, about 8 to 18 hours, which indirectly shows that the aluminum-neodymium alloy rotary sputtering target material of the invention can effectively improve the sputtering effect.
(3) The aluminum-neodymium alloy rotary sputtering targets of examples 1 to 5 have a larger reflectance and a longer oxidation resistance time than the aluminum-neodymium alloy rotary sputtering targets of examples 6 and 7, and it is found that the aluminum-neodymium alloy rotary sputtering target of the present invention has a better sputtering effect when the oxide layer has a thickness of 30 μm than when the oxide layer has a thickness of 10 μm or 50 μm. The preliminary presumption may be that the oxide layer is likely to have a film bursting phenomenon when the thickness of the oxide layer is 50 μm, and the oxide layer is likely to have cracks and crazes, which may have a certain influence on the sputtering effect. On the other hand, when the thickness is 10 μm, the sputtering effect is not greatly improved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (12)
1. The aluminum-neodymium alloy rotary sputtering target is characterized by comprising a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends which are respectively positioned on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed.
2. The aluminum-neodymium alloy rotary sputtering target according to claim 1, wherein the oxide layer has a thickness of 20 μm to 35 μm.
3. The preparation method of the aluminum-neodymium alloy rotary sputtering target is characterized by comprising the following steps of:
uniformly mixing 95-99.9% of aluminum and 0.1-5% of neodymium according to atomic percentage, smelting, and then sequentially casting, molding, extruding and annealing to obtain a precursor;
carrying out surface hard oxidation treatment on the precursor to form an oxide layer on the surface of the precursor, and then carrying out machining treatment to obtain an aluminum-neodymium alloy rotary sputtering target; the rotary aluminum-neodymium alloy sputtering target comprises a body, wherein the outermost layer of the body is an oxide layer, the body comprises a sputtering end and mounting ends which are respectively positioned on two sides of the sputtering end, and the sputtering end and the mounting ends are integrally formed.
4. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 3, wherein the step of uniformly mixing aluminum and neodymium comprises the following steps: firstly adding aluminum ingot and then adding neodymium block.
5. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 3, wherein the smelting conditions are as follows: smelting at 1100-1200 deg.c for 20-60 min, skimming slag, mixing with refiner and stilling to obtain mixed metal liquid.
6. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 5, wherein the step of casting and molding is as follows: semi-continuously casting the smelted mixed molten metal to obtain a casting rod with a preset size; in the casting process, the casting temperature is 685-715 ℃ and the casting speed is 80-100 mm/min.
7. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 6, wherein the method further comprises a step of performing first machining treatment on the cast rod after casting and molding before extrusion treatment;
the first machining processing step comprises the following steps: and cutting off the segregation areas at the head and the tail of the cast rod and oxide skins on the outer surfaces of the segregation areas so as to reach the preset size before extrusion.
8. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 7, wherein the extrusion treatment comprises the following steps: heating the cast rod after the first machining to 320-380 ℃, heating the die and the extrusion needle to 350-450 ℃, cleaning the inner cylinder of the die before extrusion, and then maintaining the extrusion speed at 0.5-1.0 m/min until extrusion to obtain an extrusion blank with a preset size.
9. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 8, wherein the annealing treatment comprises the following steps: and (3) preserving the temperature of the extrusion blank within the temperature range of 250-400 ℃ for 2-5 h, and then cooling to obtain the extrusion blank after annealing treatment.
10. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 9, wherein the method further comprises a step of performing secondary machining on the annealed extrusion blank after annealing treatment and before surface hard oxidation treatment;
the second machining processing step comprises the following steps: and processing the two ends of the annealed extrusion blank to the size of a finished product, and processing the sputtering area of the annealed extrusion blank to leave a preset allowance to obtain a precursor.
11. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 3, wherein the surface hard oxidation treatment comprises the following steps: and treating the surface of the precursor by using acid liquor, and performing hole sealing treatment to form an oxide layer on the surface of the precursor.
12. The method for preparing the aluminum-neodymium alloy rotary sputtering target material according to claim 11, wherein the acid solution is a sulfuric acid solution or an oxalic acid solution; the acid liquor has a mass percentage concentration of 10-30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010710119.3A CN112048703A (en) | 2020-07-22 | 2020-07-22 | Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010710119.3A CN112048703A (en) | 2020-07-22 | 2020-07-22 | Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112048703A true CN112048703A (en) | 2020-12-08 |
Family
ID=73601191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010710119.3A Pending CN112048703A (en) | 2020-07-22 | 2020-07-22 | Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112048703A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959595A (en) * | 2021-12-17 | 2022-08-30 | 常州苏晶电子材料有限公司 | High-purity aluminum-neodymium alloy target material for sputtering and manufacturing method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200641171A (en) * | 2005-04-13 | 2006-12-01 | Heraeus Gmbh W C | Tub target, particularly for coating TFT LCD screens, and methods for its manufacture |
| EP2365515A1 (en) * | 2010-03-09 | 2011-09-14 | Applied Materials, Inc. | Rotatable target, backing tube, sputtering installation and method for producing a rotatable target |
| CN104831242A (en) * | 2015-04-08 | 2015-08-12 | 无锡舒玛天科新能源技术有限公司 | Large-size integral aluminum-neodymium rotary target material and preparation method thereof |
| CN105220092A (en) * | 2015-11-03 | 2016-01-06 | 基迈克材料科技（苏州）有限公司 | For the rafifinal target extrusion process method of liquid crystal flat panel display plated film |
| CN107075664A (en) * | 2014-11-07 | 2017-08-18 | 应用材料公司 | The Integral type rotary target of high performance-price ratio |
| CN107953084A (en) * | 2017-11-24 | 2018-04-24 | 韶关市欧莱高新材料有限公司 | A kind of manufacture method of rafifinal rotary target material |
-
2020
- 2020-07-22 CN CN202010710119.3A patent/CN112048703A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200641171A (en) * | 2005-04-13 | 2006-12-01 | Heraeus Gmbh W C | Tub target, particularly for coating TFT LCD screens, and methods for its manufacture |
| EP2365515A1 (en) * | 2010-03-09 | 2011-09-14 | Applied Materials, Inc. | Rotatable target, backing tube, sputtering installation and method for producing a rotatable target |
| CN107075664A (en) * | 2014-11-07 | 2017-08-18 | 应用材料公司 | The Integral type rotary target of high performance-price ratio |
| CN104831242A (en) * | 2015-04-08 | 2015-08-12 | 无锡舒玛天科新能源技术有限公司 | Large-size integral aluminum-neodymium rotary target material and preparation method thereof |
| CN105220092A (en) * | 2015-11-03 | 2016-01-06 | 基迈克材料科技（苏州）有限公司 | For the rafifinal target extrusion process method of liquid crystal flat panel display plated film |
| CN107953084A (en) * | 2017-11-24 | 2018-04-24 | 韶关市欧莱高新材料有限公司 | A kind of manufacture method of rafifinal rotary target material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959595A (en) * | 2021-12-17 | 2022-08-30 | 常州苏晶电子材料有限公司 | High-purity aluminum-neodymium alloy target material for sputtering and manufacturing method thereof |
| CN114959595B (en) * | 2021-12-17 | 2024-03-29 | 常州苏晶电子材料有限公司 | High-purity aluminum neodymium alloy target material for sputtering and manufacturing method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR102369518B1 (en) | Manufacturing method of 1XXX series negative electrode foil for aluminum electrolytic capacitor | |
| KR101523894B1 (en) | Silver alloy sputtering target for forming electroconductive film, and method for manufacturing same | |
| EP2832895B1 (en) | Silver-based cylindrical target | |
| CN101376963B (en) | Ag-based alloy sputtering target | |
| JP3993530B2 (en) | Ag-Bi alloy sputtering target and method for producing the same | |
| JP6427267B2 (en) | Aluminum alloy substrate for magnetic disk, method of manufacturing the same, and magnetic disk using the aluminum alloy substrate for magnetic disk | |
| CN111235425B (en) | AgPdCu alloy and preparation method thereof, and AgPdCu alloy sputtering target and preparation method thereof | |
| EP2034035B1 (en) | Process for producing aluminum alloy plate | |
| CN109563572B (en) | Aluminum alloy plate for magnetic disk substrate, method for producing same, and magnetic disk | |
| KR101854009B1 (en) | Silver-alloy sputtering target for conductive-film formation, and method for producing same | |
| TWI485272B (en) | Pure copper plate manufacturing methods and pure copper plate | |
| CN110592406A (en) | Preparation method of high-purity aluminum-copper alloy target blank for sputtering | |
| CN111958333A (en) | Polishing process of neodymium-aluminum target sputtering surface | |
| WO2021046927A1 (en) | Nickel-rhenium alloy rotary tubular target material containing trace rare earth elements and preparation method therefor | |
| CN112048703A (en) | Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof | |
| JP4094395B2 (en) | Titanium plate for electrolytic Cu foil production drum and production method thereof | |
| CN114934261B (en) | Iron target, iron-nickel alloy target and manufacturing method thereof | |
| KR20170026398A (en) | Aluminum sputtering target | |
| TWI684652B (en) | Copper manganese sputtering target | |
| CN113862497A (en) | AgZn target material and preparation method thereof | |
| JP2004084065A (en) | Silver alloy sputtering target and its producing method | |
| JPH11315338A (en) | Aluminum alloy for magnetic disk, excellent in zincate treatment property | |
| JP2007308767A (en) | Method for producing aluminum alloy thick plate, and aluminum alloy thick plate | |
| JP2002069626A (en) | Sputtering target and its production method | |
| CN117987777A (en) | Copper alloy sputtering film, method for producing same, copper alloy sputtering target, and method for producing same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201208 |
|
| RJ01 | Rejection of invention patent application after publication |