CN114769595A - Preparation process and application of aluminum-chromium alloy target - Google Patents
Preparation process and application of aluminum-chromium alloy target Download PDFInfo
- Publication number
- CN114769595A CN114769595A CN202210394173.0A CN202210394173A CN114769595A CN 114769595 A CN114769595 A CN 114769595A CN 202210394173 A CN202210394173 A CN 202210394173A CN 114769595 A CN114769595 A CN 114769595A
- Authority
- CN
- China
- Prior art keywords
- sheath
- treatment
- alloy target
- isostatic pressing
- aluminum
- 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
- 229910000599 Cr alloy Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000000788 chromium alloy Substances 0.000 title claims abstract description 34
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 153
- 239000000956 alloy Substances 0.000 claims abstract description 153
- 238000011282 treatment Methods 0.000 claims abstract description 138
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 70
- 238000007872 degassing Methods 0.000 claims abstract description 62
- 239000000843 powder Substances 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 43
- 238000003754 machining Methods 0.000 claims abstract description 33
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 29
- 238000011049 filling Methods 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000013077 target material Substances 0.000 claims description 74
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 26
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 21
- 238000004544 sputter deposition Methods 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 238000009434 installation Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 7
- -1 aluminum-titanium-chromium Chemical compound 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 5
- 238000002161 passivation Methods 0.000 claims description 2
- QRRWWGNBSQSBAM-UHFFFAOYSA-N alumane;chromium Chemical compound [AlH3].[Cr] QRRWWGNBSQSBAM-UHFFFAOYSA-N 0.000 claims 1
- 238000005056 compaction Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 15
- 238000005260 corrosion Methods 0.000 description 14
- 238000013461 design Methods 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- 238000003825 pressing Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000005204 segregation Methods 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 7
- 229910000838 Al alloy Inorganic materials 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000007888 film coating Substances 0.000 description 6
- 238000009501 film coating Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005457 optimization Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 239000012774 insulation material Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011900 installation process Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000013011 mating Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005058 metal casting Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- 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
- B22F3/24—After-treatment of workpieces or articles
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
- B22F2003/153—Hot isostatic pressing apparatus specific to HIP
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Abstract
The invention belongs to the technical field of target preparation, and particularly relates to a preparation process and application of an aluminum-chromium alloy target, wherein the preparation process of the target comprises the following steps of S1: preparing alloy powder; step S2: putting the prepared alloy powder into a sheath, splicing and fixing the left half block and the right half block of the sheath in a bolt and nut fixing mode, and carrying out cold isostatic pressing treatment; step S3: performing primary degassing treatment on the alloy target blank; step S4: performing primary hot isostatic pressing treatment on the alloy target blank formed in the step S3, performing secondary degassing treatment, and taking out the sheath; step S5: filling the blanks subjected to the second degassing treatment into a sheath, and performing second hot isostatic pressing treatment; step S6: taking out the pack from the blank subjected to the second hot isostatic pressing treatment, machining, cleaning and carrying out vacuum heat treatment; step S7: and modifying the surface of the alloy target obtained in the step S6 with an anticorrosive layer and a heat-insulating layer. The method has the advantages of high compactness, uniform crystal grains and better mechanical property.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a preparation process and application of an aluminum-chromium alloy target.
Background
With the rapid development of the semiconductor industry, the demand of coating materials as important materials for manufacturing semiconductor electronic devices is increasing. The target material is used as an important coating material, and the main method for preparing the film material through the target material is a Physical Vapor Deposition (PVD) method, wherein the most common method is a sputtering coating method, and the target material is widely applied to the fields of integrated circuits, flat panel displays, solar energy, optical devices and the like.
The traditional target processing technology is mainly a casting technology, particularly the casting of metal targets, mainly comprises the steps of machining an ingot, heat treatment and the like, has the advantages of low cost, easiness in forming and the like, but also has the defects of low ductility, easiness in cracking and the like of castings, and particularly has the problems of nonuniform tissues, component segregation and the like in the processing of alloy targets, so that the other processing technology commonly adopted at present is a powder metallurgy method; the method is a process technology for preparing metal materials, composite materials and various products by taking metal powder or metal powder and non-metal powder as raw materials through forming and sintering, the prepared materials generally have unique chemical composition and mechanical and physical properties, but cannot be obtained by a traditional casting method, and the method is an important way for solving the defect problems of the targets prepared by the traditional method.
According to the intensive research of the inventor, the related technologies for preparing the aluminum-chromium alloy target are relatively few, but a small number of patents disclose the preparation technologies related to the aluminum alloy target. For example: chinese patent publication No. CN 101214546a discloses a powder metallurgy preparation method of a titanium-aluminum alloy target material, which comprises the following steps: preparing titanium-aluminum alloy powder according with the component ratio by adopting an atomization method or mixing the titanium powder and the aluminum powder, then performing powder loading and cold isostatic pressing, placing the cold isostatic pressing blank into a sheath for degassing treatment, performing hot isostatic pressing sintering after degassing is finished, and finally processing to obtain the titanium-aluminum alloy target material. In the method, the titanium-aluminum alloy target material is prepared by a hot isostatic pressing process only once, the temperature is extremely high, the microstructure of a sintered product is not adjusted, and the uniformity of particles and tissues is limited; chinese patent with publication number CN 104419847A discloses a titanium-aluminum-chromium alloy target material and a preparation method thereof, wherein the target material is obtained mainly by cold isostatic pressing and hot isostatic pressing treatment, but the target material prepared by the method is difficult to be rapidly removed from a sheath, and the surface of the target material is not subjected to further antiseptic treatment, so that the surface property of the target material is difficult to be well ensured; the Chinese patent with the application number of CN 113564544A also discloses an aluminum alloy target and a preparation method thereof, but the method can prepare the alloy target with compact structure, but the sheath structure and the like are not reasonably designed, so that the sheath assembling and taking are troublesome in the preparation process, and the production efficiency is influenced.
Based on the above, the application provides a preparation process and application of an aluminum-chromium alloy target, and the technical problems of insufficient target compactness, inconvenient sheath assembly and disassembly and the like in the prior art are effectively solved through reasonable improvement design of the target preparation process, so that the defects and shortcomings in the prior art are avoided.
Disclosure of Invention
The invention aims to: aiming at the problems existing at present, the preparation process and the application of the aluminum-chromium alloy target are provided, and the technical problems of insufficient target compactness, inconvenient sheath assembly and taking and the like in the prior art are effectively solved through reasonable improvement and design of the target preparation process, so that the defects and shortcomings in the prior art are avoided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation process of an aluminum-chromium alloy target material comprises the following specific steps:
step S1: preparing alloy powder;
step S2: putting the prepared alloy powder into a sheath, splicing and fixing the left half block and the right half block of the sheath in a bolt and nut fixing mode, and carrying out cold isostatic pressing treatment;
step S3: performing first degassing treatment on the alloy target blank formed in the step S2;
step S4: performing first hot isostatic pressing treatment on the alloy target blank formed in the step S3, performing second degassing treatment, and taking out the sheath;
step S5: filling the blank subjected to the second degassing treatment into a jacket, and performing second hot isostatic pressing treatment;
step S6: taking the blank subjected to the second hot isostatic pressing treatment out of the sheath, performing machining and cleaning treatment, and performing vacuum heat treatment;
step S7: and (5) modifying the surface of the alloy target obtained in the step S6 with an anticorrosive layer and a heat-insulating layer to obtain the required alloy target finished product.
Preferably, in step S1, the alloy powder comprises the following components by mass percent: 70-85% of simple substance aluminum powder with the purity of 3N-5N and 15-30% of simple substance chromium powder with the purity of 3N-5N; the average grain diameter of the alloy powder is 35-100 mu m; and mixing the simple substance aluminum powder and the simple substance chromium powder for 48-72 h under the atmosphere of inert gas protection to form alloy powder. The purity of the simple substance aluminum powder and the simple substance chromium powder is regulated, so that the performance and the quality of the prepared alloy target material are ensured; the grain size of the alloy powder is limited, so that the compactness and the grain uniformity of a target sample after the target is manufactured are guaranteed; the mixing is carried out in an inert atmosphere, on one hand, in order to ensure that the aluminum powder or the chromium powder is influenced by oxidizing gas to cause oxidation and the like in the mixing process, on the other hand, the aluminum powder and the chromium powder are uniformly mixed in a mixing mode, and the uniform alloy components are obtained after the target material is prepared.
Preferably, in the step S2, the jacket fixes the fixing block by a bolt and a nut, so that the left half block and the right half block are spliced into an integral jacket; then, filling alloy powder into an internal forming groove of a sheath, compacting, and then carrying out cold isostatic pressing treatment; the pressure of the cold isostatic pressing treatment is 100 MPa-180 MPa, and the pressure maintaining time of cold forming is 15 min-20 min. The alloy powder is formed for the first time in a cold isostatic pressing mode, cold pressing combination between the alloy powder is mainly achieved in a physical mode, cold pressing blanks are formed, and convenience is provided for subsequent hot isostatic pressing treatment.
Preferably, in the step S3, the temperature of the first degassing treatment is 300 to 400 ℃, and the degassing time is 10 to 20 hours; first degassing partThe vacuum degree during treatment is controlled at 10-2Pa～10-4In the Pa range. The purpose of the degassing treatment is: the compactness of the blank is improved through the process.
Preferably, in the step S4, the temperature of the first hot isostatic pressing treatment is 300 ℃ to 400 ℃; the pressure of the first hot isostatic pressing treatment is 150 MPa-300 MPa; the time of the first hot isostatic pressing treatment is 12-24 hours; after the first hot isostatic pressing treatment is finished, cooling and pressure relief are carried out; then continuing to perform secondary degassing treatment, wherein the temperature of the secondary degassing treatment is 400-600 ℃, and the degassing time is 15-30 h; the vacuum degree in the second degassing treatment was controlled to 10-2Pa～10-4In the Pa range. After the hot isostatic pressing treatment, the atomic motion intensity among alloy particles of the target blank can be improved in a high-temperature mode, so that the alloy particles are further compactly combined, and the preparation of the high-compactness alloy target is facilitated.
Preferably, in the step S5, the holding temperature of the second hot isostatic pressing treatment is 1000 ℃ to 1200 ℃; the heat preservation time is 3 h-6 h, and the pressure maintaining pressure is 300 MPa-450 MPa. And performing hot isostatic pressing again, wherein the main purpose is to further improve the compactness of the formed target.
Preferably, in step S6, the alloy target surface is subjected to finish machining and mounting hole machining by a machining method, cleaned, and then subjected to vacuum heat treatment; the vacuum heat treatment is carried out in a vacuum sintering furnace, the temperature of the vacuum heat treatment is 400-600 ℃, and the pressure of the vacuum heat treatment is 10-3Pa～10-5Pa, and the time of vacuum heat treatment is 15-30 h. The precision quality of the surface of the alloy target material can be guaranteed by the mechanical finish machining of the surface; through vacuum heat treatment, the microstructure optimization and grain refinement of the alloy target are facilitated, the component segregation is reduced, and the method has a positive effect on ensuring the integral surface quality and mechanical property of the alloy target.
Preferably, the structure of the alloy target comprises a disc-shaped sputtering block protruding outwards and a mounting ring; the surface of the mounting ring is decorated with an anticorrosive layer and a heat insulation layer, and the surface of the heat insulation layer is plated with an alloy passivation film; the diameter of the mounting ring is larger than that of the sputtering block, and a plurality of mounting holes are formed in the mounting ring in an array mode. The structural design of the alloy target material can realize the surface coating function through the sputtering block on one hand, and the design of the mounting ring and the mounting hole on the other hand is beneficial to the target material to adapt to the mounting of different clamping tools, thereby ensuring the sputtering coating efficiency of the target material; the arrangement of the anticorrosive coating and the heat-insulating layer aims to improve the corrosion resistance of the target material, on one hand, the part of the target material is frequently installed and disassembled particularly at the position of the installation ring, the part of the target material is frequently contacted with a clamp, and the position of the installation ring is also frequently held by hands in the installation process, so that the corrosion defect can be caused by being contaminated by corrosive substances, the anticorrosive coating is modified or plated, and the target material corrosion is favorably avoided and the service life of the target material is prolonged; through the arrangement of the heat insulation layer, the influence of heat generated in the sputtering coating working process of the target on the clamp is mainly reduced, so that the installation precision is insufficient or the thermal expansion deformation of the clamp is caused; the anticorrosive coating and the thermal insulation layer are only arranged on the mounting ring, and the anticorrosive coating and the thermal insulation layer are not arranged on the surface of the sputtering block, so that the film coating condition of anticorrosive materials and thermal insulation materials is mainly avoided from being caused in the actual sputtering film coating process, and the film coating quality is prevented from being influenced by the anticorrosive coating and the thermal insulation materials.
Preferably, the sheath comprises two half blocks, and the sheath is formed by splicing the two half blocks; a forming groove matched with the shape of the alloy target is formed in the sheath; the splicing surface of the left half block of the sheath is provided with an outward convex matching bulge, and the splicing surface of the right half block of the sheath is provided with an inward concave matching groove; the right end of the left half block of the sheath is provided with a hinge block, the left end of the right half block of the sheath is provided with a hinge frame matched with the hinge block, an installation shaft is fixedly welded in the hinge frame, a shaft hole matched with the installation shaft is formed in the matching bulge, and the installation shaft penetrates through the shaft hole to realize the hinge joint of the left half block and the right half block of the sheath; the other one end of the left half block and the other one end of the right half block of the sheath are both provided with fixed blocks, and fixing holes for locking and fixing the sheath are formed in the fixed blocks.
Through the structural design of the sheath, the following operation functions can be realized: the sheath is divided into two halves, so that the target material in the sheath can be conveniently taken out or put in; the sheath can be spliced into a complete disc-shaped sleeve body by rotating the hinge block and the hinge frame; a forming groove matched with the target material in shape is formed in the sheath, so that alloy powder or a target material blank can be conveniently loaded; the fixing blocks on the two half blocks are fastened through bolts and nuts, and the matching protrusions are embedded into the matching grooves at the moment; after cold isostatic pressing or hot isostatic pressing, the interaction force between the target and the sheath is larger, the target can be taken out only by applying larger force in the traditional sheath structure, the traditional sheath structure is relatively troublesome, and the surface of the target is easily damaged in the taking-out process; by adopting the sheath structure, only the bolt and the nut at the position of the fixed block need to be loosened, so that the two half parts of the sheath can be opened towards two sides with smaller force, the target can be easily taken out at the moment, and the target surface is ensured to be intact.
Preferably, the preparation process is used for producing and preparing the aluminum-titanium-chromium alloy target, the aluminum-titanium alloy target and the aluminum-chromium alloy target.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
on one hand, the technical scheme of the application can obtain the alloy target material with higher compactness and better grain uniformity, and the alloy target material has no air holes and component segregation, has better machining performance and higher overall quality, and can meet the use requirement of the sputtering target material.
On the other hand, the anti-corrosion layer and the heat insulation layer are arranged at the position of the mounting ring, so that on one hand, the surface anti-corrosion performance of the mounting ring is improved, the heat insulation effect between the mounting ring and the clamp is ensured, and the clamp is prevented from expanding or thermally deforming due to heat generated in the sputtering process; due to the design of the mounting ring and the mounting hole, the target is suitable for mounting different clamps, and the application range of the target is favorably widened.
On the other hand, the alloy powder or the alloy blank can be conveniently assembled and disassembled and taken out through the structural design of the sheath and the action of the sheath, compared with the conventional traditional sleeve packaging structure, the sleeve packaging structure is convenient to assemble and disassemble, and the surface quality of the target cannot be influenced in the process of taking out the target; the alloy target preparation process is suitable for production and preparation of aluminum-titanium-chromium alloy targets, aluminum-titanium alloy targets and aluminum-chromium alloy targets, and has good practical value and popularization value.
Drawings
FIG. 1 is a schematic view of the outline structure of an Al-Cr alloy target according to the present invention;
FIG. 2 is a schematic view of a jacket deployment configuration of the present invention;
FIG. 3 is a schematic top view of a jacket according to the present invention;
FIG. 4 is a schematic cross-sectional view of the aluminum-chromium alloy target of the present invention.
In the figure: 1. sputtering block; 2. a mounting ring; 3. mounting holes; 4. forming a groove; 5. sheathing; 6. a mating groove; 7. a mating protrusion; 8. a hinged frame; 9. installing a shaft; 10. a hinged block; 11. a fixed block; 12. a fixing hole; 13. an anticorrosive layer; 14. an insulating layer.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the technical solutions in the embodiments of the present invention will be described below with reference to the drawings in the embodiments of the present invention, it is obvious that the described embodiments are some, but not all embodiments of the present invention, and based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
Example 1, as shown in figures 1-4:
a preparation process of an aluminum-chromium alloy target material comprises the following specific steps:
step S1: preparing alloy powder;
step S2: putting the prepared alloy powder into a sheath 5, splicing and fixing the left half block and the right half block of the sheath 5 in a bolt and nut fixing mode, and carrying out cold isostatic pressing treatment;
step S3: performing first degassing treatment on the alloy target blank formed in the step S2;
step S4: performing first hot isostatic pressing treatment on the alloy target blank formed in the step S3, performing second degassing treatment, and taking out the sheath 5;
step S5: filling the preform subjected to the second degassing treatment into the sheath 5, and performing second hot isostatic pressing treatment;
step S6: taking the blank subjected to the second hot isostatic pressing treatment out of the sheath 5, carrying out machining and cleaning treatment, and carrying out vacuum heat treatment;
step S7: and (4) modifying the surface of the alloy target obtained in the step S6 with an anticorrosive layer 13 and a heat insulation layer 14 to obtain a required alloy target finished product.
Preferably, in step S1, the alloy powder comprises the following components by mass percent: 70-85% of simple substance aluminum powder with the purity of 3N-5N and 15-30% of simple substance chromium powder with the purity of 3N-5N; the average grain diameter of the alloy powder is 35-100 mu m; and mixing the elemental aluminum powder and the elemental chromium powder for 48-72 h under the inert gas protection atmosphere to form alloy powder. The purity of the elemental aluminum powder and the elemental chromium powder is regulated, so that the performance and the quality of the prepared alloy target material are ensured; the grain size of the alloy powder is limited, so that the compactness and the grain uniformity of a target material sample after the target material is prepared are guaranteed; the mixing is carried out in an inert atmosphere, on one hand, in order to ensure that the aluminum powder or the chromium powder is influenced by oxidizing gas to cause oxidation and the like in the mixing process, on the other hand, the aluminum powder and the chromium powder are uniformly mixed in a mixing mode, and the uniform alloy components are obtained after the target material is prepared.
Preferably, in the step S2, the jacket 5 fixes the fixed block 11 by a bolt and a nut, so that the left half block and the right half block are spliced into an integral jacket 5; then the alloy powder is put into an internal forming groove 4 of a sheath 5 to be compacted, and then cold isostatic pressing treatment is carried out; the pressure of the cold isostatic pressing treatment is 100 MPa-180 MPa, and the pressure maintaining time of cold forming is 15 min-20 min. The alloy powder is formed for the first time in a cold isostatic pressing mode, cold pressing combination between the alloy powder is mainly achieved in a physical mode, cold pressing blanks are formed, and convenience is provided for subsequent hot isostatic pressing treatment.
Preferably, in the step S3, the temperature of the first degassing treatment is 300 to 400 ℃, and the degassing time is 10 to 20 hours; the vacuum degree in the first degassing treatment was controlled to 10-2Pa～10-4In the Pa range. The purpose of the degassing treatment is: the compactness of the blank is improved through the process.
Preferably, in the step S4, the temperature of the first hot isostatic pressing treatment is 300 ℃ to 400 ℃; the pressure of the first hot isostatic pressing treatment is 150 MPa-300 MPa; the time of the first hot isostatic pressing treatment is 12-24 hours; after the first hot isostatic pressing treatment is finished, cooling and pressure relief are carried out; then continuing to perform secondary degassing treatment at the temperature of 400-600 ℃ for 15-30 h; the vacuum degree in the second degassing treatment was controlled to 10-2Pa～10-4In the Pa range. After the hot isostatic pressing treatment, the atomic motion intensity among alloy particles of the target blank can be improved in a high-temperature mode, so that the alloy particles are further compactly combined, and the preparation of the high-compactness alloy target is facilitated.
Preferably, in the step S5, the holding temperature of the second hot isostatic pressing treatment is 1000 ℃ to 1200 ℃; the heat preservation time is 3 h-6 h, and the pressure maintaining pressure is 300 MPa-450 MPa. And performing hot isostatic pressing again, wherein the main purpose is to further improve the compactness of the formed target.
Preferably, in step S6, the surface of the alloy target material is subjected to finish machining and machining of the mounting hole 3 by a machining method, and is cleaned and then subjected to vacuum heat treatment; the vacuum heat treatment is carried out in a vacuum sintering furnace, the temperature of the vacuum heat treatment is 400-600 ℃, and the pressure of the vacuum heat treatment is 10-3Pa～10-5Pa, and the time of vacuum heat treatment is 15-30 h. The mechanical finish machining of the surface is beneficial to ensuring the precision and quality of the surface of the alloy target material; through vacuum heat treatment, the microstructure optimization and grain refinement of the alloy target are facilitated, the component segregation is reduced, and the method has a positive effect on ensuring the integral surface quality and mechanical property of the alloy target.
Preferably, the structure of the alloy target comprises a disc-shaped sputtering block 1 and a mounting ring 2 which are protruded outwards; the surface of the mounting ring 2 is decorated with an anticorrosive layer 13 and a heat insulation layer 14, and the surface of the heat insulation layer 14 is plated with an alloy passive film; the diameter of the mounting ring 2 is larger than that of the sputtering block 1, and a plurality of mounting holes 3 are formed in the mounting ring 2 in an array mode. The structural design of the alloy target material can realize the surface coating function through the sputtering block 1 on one hand, and on the other hand, the design of the mounting ring 2 and the mounting hole 3 is beneficial to the target material to adapt to the mounting of different clamping tools, thereby ensuring the sputtering coating efficiency of the target material; the arrangement of the anticorrosive coating 13 and the heat-insulating layer 14 is to improve the corrosion resistance of the target material, on one hand, especially at the position of the mounting ring 2, the position of the target material is frequently installed and disassembled, the contact between the position of the target material and a clamp is frequent, and in the installation process, the position of the mounting ring 2 is also frequently held by hands, so that the corrosion defect can occur due to the contamination of corrosive substances, the anticorrosive coating 13 is decorated or plated, and the target material corrosion can be avoided, and the service life of the target material can be prolonged; the arrangement of the heat insulation layer 14 is mainly used for reducing the influence of heat generated in the sputtering coating working process of the target on the clamp, so that the mounting precision is not enough or the thermal expansion deformation of the clamp is caused; the anti-corrosion layer 13 and the heat insulation layer 14 are only arranged on the mounting ring 2, and the anti-corrosion layer 13 and the heat insulation layer 14 are not arranged on the surface of the sputtering block 1, so that the film coating condition of anti-corrosion materials and heat insulation materials in the actual sputtering film coating process is avoided, and the film coating quality is prevented from being influenced by the anti-corrosion materials and the heat insulation materials.
Preferably, the sheath 5 comprises two half blocks, and the sheath 5 is formed by splicing the two half blocks; a forming groove 4 matched with the shape of the alloy target is formed in the sheath 5; the left half block splicing surface of the sheath 5 is provided with an outward convex matching bulge 7, and the right half block splicing surface of the sheath 5 is provided with an inward concave matching groove 6; the right end of the left half of the sheath 5 is provided with a hinge block 10, the left end of the right half of the sheath 5 is provided with a hinge frame 8 matched with the hinge block 10, an installation shaft 9 is fixedly welded in the hinge frame 8, a shaft hole matched with the installation shaft 9 is formed in the matching bulge 7, and the installation shaft 9 penetrates through the shaft hole to realize the hinge joint of the left half and the right half of the sheath 5; the other ends of the left half block and the right half block of the sheath 5 are provided with fixing blocks 11, and fixing holes 12 used for locking and fixing the sheath 5 are formed in the fixing blocks 11.
By means of the structural design of the sheath 5, the following operating functions can be achieved: the sheath 5 is divided into two halves, so that the target material in the sheath 5 can be conveniently taken out or put in; the sheath 5 can be spliced into a complete disc-shaped sleeve body by rotating the hinge block 10 and the hinge frame 8; a forming groove 4 matched with the target material in shape is formed in the sheath 5, so that alloy powder or a target material blank can be conveniently loaded; the fixing block 11 on the two half blocks is fastened by the sheath 5 through bolts and nuts, and the matching protrusion 7 is embedded into the matching groove 6; after cold isostatic pressing or hot isostatic pressing, the interaction force between the target material and the sheath 5 is larger, the target material can be taken out only by applying larger force to the traditional sheath 5 structure, the operation is relatively troublesome, and the surface of the target material is easily damaged in the taking-out process; by adopting the sheath 5 structure, only the bolts and the nuts at the positions of the fixed blocks 11 need to be loosened, so that the two half blocks of the sheath 5 can be opened towards two sides with smaller force, the target can be taken out easily, and the target surface is ensured to be intact.
Preferably, the preparation process is used for producing and preparing the aluminum-titanium-chromium alloy target, the aluminum-titanium alloy target and the aluminum-chromium alloy target.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
on one hand, the technical scheme of the application can obtain the alloy target material with higher compactness and better grain uniformity, and the alloy target material has no air holes and component segregation, has better machining performance and higher overall quality, and can meet the use requirement of the sputtering target material.
On the other hand, the anti-corrosion layer 13 and the heat insulation layer 14 are arranged at the position of the mounting ring 2, so that on one hand, the surface anti-corrosion performance of the mounting ring is improved, the heat insulation effect between the mounting ring 2 and the clamp is ensured, and the clamp is prevented from expanding or thermally deforming due to heat generated in the sputtering process; due to the design of the mounting ring 2 and the mounting hole 3, the target material is suitable for mounting different clamps, and the application range of the target material is favorably widened.
On the other hand, the alloy powder or the blank can be conveniently loaded and unloaded and taken out by the structural design of the sheath 5 and the action of the sheath 5, compared with the traditional sheath 5 structure, the structure is convenient to assemble and disassemble, and the surface quality of the target cannot be influenced in the process of taking out the target; the preparation process of the alloy target is suitable for production and preparation of the aluminum-titanium-chromium alloy target, the aluminum-titanium alloy target and the aluminum-chromium alloy target, and has good practical value and popularization value.
Specific example 2, as shown in fig. 1-4:
a preparation process of an aluminum-chromium alloy target material comprises the following specific steps:
step S1: preparing alloy powder;
step S2: putting the prepared alloy powder into a sheath 5, splicing and fixing the left half block and the right half block of the sheath 5 in a bolt and nut fixing mode, and carrying out cold isostatic pressing treatment;
step S3: performing first degassing treatment on the alloy target blank formed in the step S2;
step S4: performing primary hot isostatic pressing treatment on the alloy target blank formed in the step S3, performing secondary degassing treatment, and taking out the sheath 5;
step S5: filling the blank subjected to the second degassing treatment into a jacket 5, and performing second hot isostatic pressing treatment;
step S6: taking the pack 5 out of the blank subjected to the second hot isostatic pressing treatment, machining, cleaning and carrying out vacuum heat treatment;
step S7: modifying the anticorrosive layer 13 and the heat-insulating layer 14 on the surface of the alloy target obtained in the step S6 to obtain a required alloy target finished product.
Preferably, in step S1, the alloy powder comprises the following components by mass percent: 70% of simple substance aluminum powder with the purity of 3N and 30% of simple substance chromium powder with the purity of 3N; the average grain diameter of the alloy powder is 35 μm; and mixing the elemental aluminum powder and the elemental chromium powder for 48 hours under the inert gas protection atmosphere to form alloy powder. The purity of the simple substance aluminum powder and the simple substance chromium powder is regulated, so that the performance and the quality of the prepared alloy target material are ensured; the grain size of the alloy powder is limited, so that the compactness and the grain uniformity of a target sample after the target is manufactured are guaranteed; the mixing is carried out in an inert atmosphere, on one hand, in order to ensure that the aluminum powder or the chromium powder is influenced by oxidizing gas to cause oxidation and the like in the mixing process, on the other hand, the aluminum powder and the chromium powder are uniformly mixed in a mixing mode, and the uniform alloy components are obtained after the target material is prepared.
Preferably, in the step S2, the sheath 5 fixes the fixed block 11 by a bolt and a nut, so that the left half block and the right half block are combined into an integral sheath 5; then, filling alloy powder into an internal forming groove 4 of a sheath 5, compacting, and then carrying out cold isostatic pressing treatment; the pressure of the cold isostatic pressing treatment is 100MPa, and the pressure maintaining time of cold forming is 15 min. The alloy powder is formed for the first time in a cold isostatic pressing mode, cold pressing combination between the alloy powder is mainly achieved through a physical mode, cold pressing blanks are formed, and convenience is brought to subsequent hot isostatic pressing treatment.
Preferably, in the step S3, the temperature of the first degassing treatment is 300 ℃, and the degassing time is 10 hours; the vacuum degree in the first degassing treatment was controlled to 10-2Pa. The purpose of the degassing treatment is: the compactness of the blank is improved through the process.
Preferably, in the step S4, the temperature of the first hot isostatic pressing treatment is 300 ℃; the pressure of the first hot isostatic pressing treatment is 150 MPa; the time of the first hot isostatic pressing treatment is 12 hours; after the first hot isostatic pressing treatment is finished, cooling and pressure relief are carried out; then continuing to perform secondary degassing treatment at 400 ℃ for 15 h; the vacuum degree in the second degassing treatment was controlled to 10-2Pa. After the hot isostatic pressing treatment, the target blank can improve the intensity of atomic motion among alloy particles in a high-temperature mode, so that further dense combination among the alloy particles is promoted, and the preparation of the high-compactness alloy target is facilitated.
Preferably, in the step S5, the holding temperature of the second hot isostatic pressing treatment is 1000 ℃; the heat preservation time is 3h, and the pressure maintaining pressure is 300 MPa. And performing hot isostatic pressing again, wherein the main purpose is to further improve the compactness of the formed target.
Preferably, in step S6, the alloy target surface is subjected to finish machining and machining of the mounting hole 3 by a machining method, and then vacuum heat treatment is performed after the alloy target surface is cleaned; the vacuum heat treatment is carried out in a vacuum sintering furnace, the temperature of the vacuum heat treatment is 400 ℃, and the pressure of the vacuum heat treatment is 10-3Pa, and the time of vacuum heat treatment is 15 h. The mechanical finish machining of the surface is beneficial to ensuring the precision and quality of the surface of the alloy target material; through vacuum heat treatment, the microstructure optimization and grain refinement of the alloy target are facilitated, the component segregation is reduced, and the method has an active effect on ensuring the overall surface quality and mechanical properties of the alloy target.
Specific example 3, as shown in fig. 1-4:
a preparation process of an aluminum-chromium alloy target material comprises the following specific steps:
step S1: preparing alloy powder;
step S2: putting the prepared alloy powder into a sheath 5, splicing and fixing the left half block and the right half block of the sheath 5 in a bolt and nut fixing mode, and carrying out cold isostatic pressing treatment;
step S3: performing first degassing treatment on the alloy target blank formed in the step S2;
step S4: performing primary hot isostatic pressing treatment on the alloy target blank formed in the step S3, performing secondary degassing treatment, and taking out the sheath 5;
step S5: filling the preform subjected to the second degassing treatment into the sheath 5, and performing second hot isostatic pressing treatment;
step S6: taking the blank subjected to the second hot isostatic pressing treatment out of the sheath 5, carrying out machining and cleaning treatment, and carrying out vacuum heat treatment;
step S7: modifying the anticorrosive layer 13 and the heat-insulating layer 14 on the surface of the alloy target obtained in the step S6 to obtain a required alloy target finished product.
Preferably, in step S1, the alloy powder comprises the following components by mass percent: 80% of simple substance aluminum powder with the purity of 4N and 20% of simple substance chromium powder with the purity of 4N; the average grain diameter of the alloy powder is 50 μm; and mixing the simple substance aluminum powder and the simple substance chromium powder for 60 hours under the atmosphere of inert gas protection to form alloy powder. The purity of the elemental aluminum powder and the elemental chromium powder is regulated, so that the performance and the quality of the prepared alloy target material are ensured; the grain size of the alloy powder is limited, so that the compactness and the grain uniformity of a target sample after the target is manufactured are guaranteed; the aluminum powder and the chromium powder are uniformly mixed in a mixing mode to ensure that uniform alloy components are obtained after the target material is prepared.
Preferably, in the step S2, the jacket 5 fixes the fixed block 11 by a bolt and a nut, so that the left half block and the right half block are spliced into an integral jacket 5; then, filling alloy powder into an internal forming groove 4 of a sheath 5, compacting, and then carrying out cold isostatic pressing treatment; the pressure of the cold isostatic pressing treatment is 150MPa, and the pressure maintaining time of cold forming is 18 min. The alloy powder is formed for the first time in a cold isostatic pressing mode, cold pressing combination between the alloy powder is mainly achieved in a physical mode, cold pressing blanks are formed, and convenience is provided for subsequent hot isostatic pressing treatment.
Preferably, in the step S3, the temperature of the first degassing treatment is 350 ℃, and the degassing time is 15 h; the vacuum degree in the first degassing treatment was controlled to 10-3Pa. The purpose of the degassing treatment is: the compactness of the blank is improved through the process.
Preferably, in the step S4, the temperature of the first hot isostatic pressing treatment is 350 ℃; the pressure of the first hot isostatic pressing treatment is 200 MPa; the time of the first hot isostatic pressing treatment is 20 h; after the first hot isostatic pressing treatment is finished, cooling and pressure relief are carried out; then continuing to perform secondary degassing treatment at the temperature of 500 ℃ for 20 h; the vacuum degree in the second degassing treatment was controlled to 10-3Pa. After the hot isostatic pressing treatment, the target blank can be processed by a high-temperature modeThe violent degree of atomic motion among the alloy particles is improved, so that the alloy particles are promoted to be further compactly combined, and the preparation of the high-compactness alloy target material is facilitated.
Preferably, in the step S5, the holding temperature of the second hot isostatic pressing treatment is 1100 ℃; the heat preservation time is 5h, and the pressure is 400 MPa. And performing hot isostatic pressing again, wherein the main purpose is to further improve the compactness of the formed target.
Preferably, in step S6, the alloy target surface is subjected to finish machining and machining of the mounting hole 3 by a machining method, and then vacuum heat treatment is performed after the alloy target surface is cleaned; the vacuum heat treatment is carried out in a vacuum sintering furnace, the temperature of the vacuum heat treatment is 500 ℃, and the pressure of the vacuum heat treatment is 10-4Pa, and the time of vacuum heat treatment is 20 h. The mechanical finish machining of the surface is beneficial to ensuring the precision and quality of the surface of the alloy target material; through vacuum heat treatment, the microstructure optimization and grain refinement of the alloy target are facilitated, the component segregation is reduced, and the method has an active effect on ensuring the overall surface quality and mechanical properties of the alloy target.
Example 4, as shown in fig. 1-4:
a preparation process of an aluminum-chromium alloy target material comprises the following specific steps:
step S1: preparing alloy powder;
step S2: putting the prepared alloy powder into a sheath 5, splicing and fixing the left half block and the right half block of the sheath 5 in a bolt and nut fixing mode, and carrying out cold isostatic pressing treatment;
step S3: performing first degassing treatment on the alloy target blank formed in the step S2;
step S4: performing primary hot isostatic pressing treatment on the alloy target blank formed in the step S3, performing secondary degassing treatment, and taking out the sheath 5;
step S5: filling the preform subjected to the second degassing treatment into the sheath 5, and performing second hot isostatic pressing treatment;
step S6: taking the blank subjected to the second hot isostatic pressing treatment out of the sheath 5, carrying out machining and cleaning treatment, and carrying out vacuum heat treatment;
step S7: and (4) modifying the surface of the alloy target obtained in the step S6 with an anticorrosive layer 13 and a heat insulation layer 14 to obtain a required alloy target finished product.
Preferably, in step S1, the alloy powder comprises the following components by mass percent: 85% of simple substance aluminum powder with the purity of 5N and 15% of simple substance chromium powder with the purity of 5N; the average grain diameter of the alloy powder is 100 mu m; and mixing the elemental aluminum powder and the elemental chromium powder for 72 hours under the inert gas protection atmosphere to form alloy powder. The purity of the elemental aluminum powder and the elemental chromium powder is regulated, so that the performance and the quality of the prepared alloy target material are ensured; the grain size of the alloy powder is limited, so that the compactness and the grain uniformity of a target material sample after the target material is prepared are guaranteed; the aluminum powder and the chromium powder are uniformly mixed in a mixing mode to ensure that uniform alloy components are obtained after the target material is prepared.
Preferably, in the step S2, the jacket 5 fixes the fixed block 11 by a bolt and a nut, so that the left half block and the right half block are spliced into an integral jacket 5; then the alloy powder is put into an internal forming groove 4 of a sheath 5 to be compacted, and then cold isostatic pressing treatment is carried out; the pressure of the cold isostatic pressing treatment is 180MPa, and the pressure maintaining time of cold forming is 20 min. The alloy powder is formed for the first time in a cold isostatic pressing mode, cold pressing combination between the alloy powder is mainly achieved in a physical mode, cold pressing blanks are formed, and convenience is provided for subsequent hot isostatic pressing treatment.
Preferably, in the step S3, the temperature of the first degassing treatment is 400 ℃, and the degassing time is 20 h; the vacuum degree during the first degassing treatment was controlled to 10-4In the Pa range. The purpose of the degassing treatment is: the compactness of the blank is improved through the process.
Preferably, in the step S4, the temperature of the first hot isostatic pressing treatment is 400 ℃; the pressure of the first hot isostatic pressing treatment is 300 MPa; the time of the first hot isostatic pressing treatment is 24 hours; first heat, etcAfter the static pressure treatment is finished, cooling and releasing pressure; then continuing to perform secondary degassing treatment at the temperature of 600 ℃ for 30 h; the vacuum degree during the second degassing treatment was controlled to 10-4Pa. After the hot isostatic pressing treatment, the atomic motion intensity among alloy particles of the target blank can be improved in a high-temperature mode, so that the alloy particles are further compactly combined, and the preparation of the high-compactness alloy target is facilitated.
Preferably, in the step S5, the holding temperature of the second hot isostatic pressing treatment is 1200 ℃; the heat preservation time is 6h, and the pressure maintaining pressure is 450 MPa. And performing hot isostatic pressing again, wherein the main purpose is to further improve the compactness of the formed target.
Preferably, in step S6, the surface of the alloy target material is subjected to finish machining and machining of the mounting hole 3 by a machining method, and is cleaned and then subjected to vacuum heat treatment; the vacuum heat treatment is carried out in a vacuum sintering furnace, the temperature of the vacuum heat treatment is 600 ℃, and the pressure of the vacuum heat treatment is 10-5Pa, and the time of vacuum heat treatment is 30 h. The precision quality of the surface of the alloy target material can be guaranteed by the mechanical finish machining of the surface; through vacuum heat treatment, the microstructure optimization and grain refinement of the alloy target are facilitated, the component segregation is reduced, and the method has an active effect on ensuring the overall surface quality and mechanical properties of the alloy target.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and shall cover the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation process of an aluminum-chromium alloy target material is characterized by comprising the following steps: the method comprises the following specific steps:
step S1: preparing alloy powder;
step S2: the prepared alloy powder is filled into a sheath (5), the left half block and the right half block of the sheath (5) are spliced and fixed in a bolt and nut fixing mode, and cold isostatic pressing treatment is carried out;
step S3: performing first degassing treatment on the alloy target blank formed in the step S2;
step S4: carrying out the first hot isostatic pressing treatment on the alloy target blank formed in the step S3, carrying out the second degassing treatment, and taking out the sheath (5);
step S5: filling the blanks subjected to the second degassing treatment into a sheath (5), and performing second hot isostatic pressing treatment;
step S6: taking the blank subjected to the second hot isostatic pressing treatment out of the sheath (5), machining, cleaning and carrying out vacuum heat treatment;
step S7: and (4) modifying the surface of the alloy target obtained in the step S6 with an anticorrosive layer (13) and a heat-insulating layer (14) to obtain a required alloy target finished product.
2. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: in the step S1, the alloy powder comprises the following components by mass percent: 70-85% of simple substance aluminum powder with the purity of 3N-5N and 15-30% of simple substance chromium powder with the purity of 3N-5N; the average grain diameter of the alloy powder is 35-100 mu m; and mixing the elemental aluminum powder and the elemental chromium powder for 48-72 h under the inert gas protection atmosphere to form alloy powder.
3. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: in the step S2, the sheath (5) firstly fixes the fixed block through a bolt and a nut, so that the left half block and the right half block are spliced into an integral sheath (5); then, filling the alloy powder into an internal forming groove (4) of a sheath (5) for compaction, and then carrying out cold isostatic pressing treatment; the pressure of the cold isostatic pressing treatment is 100 MPa-180 MPa, and the pressure maintaining time of cold forming is 15 min-20 min.
4. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: in the step S3, the first degassing treatmentThe temperature of the reaction kettle is 300-400 ℃, and the degassing time is 10-20 h; the vacuum degree in the first degassing treatment was controlled to 10-2Pa～10-4Pa range.
5. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: in the step S4, the temperature of the first hot isostatic pressing treatment is 300-400 ℃; the pressure of the first hot isostatic pressing treatment is 150 MPa-300 MPa; the time of the first hot isostatic pressing treatment is 12-24 hours; after the first hot isostatic pressing treatment is finished, cooling and pressure relief are carried out; then continuing to perform secondary degassing treatment, wherein the temperature of the secondary degassing treatment is 400-600 ℃, and the degassing time is 15-30 h; the vacuum degree during the second degassing treatment was controlled to 10-2Pa～10-4Pa range.
6. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: in the step S5, the heat preservation temperature of the second hot isostatic pressing treatment is 1000-1200 ℃; the heat preservation time is 3 h-6 h, and the pressure maintaining pressure is 300 MPa-450 MPa.
7. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: in the step S6, the surface of the alloy target material is subjected to finish machining and mounting hole (3) machining in a machining mode, and vacuum heat treatment is carried out after the alloy target material is cleaned; the vacuum heat treatment is carried out in a vacuum sintering furnace, the temperature of the vacuum heat treatment is 400-600 ℃, and the pressure of the vacuum heat treatment is 10-3Pa～10-5Pa, and the time of vacuum heat treatment is 15-30 h.
8. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: the structure of the alloy target comprises a disc-shaped sputtering block (1) protruding outwards and a mounting ring (2); the surface of the mounting ring (2) is decorated with an anticorrosive layer (13) and a heat insulation layer (14), and the surface of the heat insulation layer (14) is plated with an alloy passivation film; the diameter of the mounting ring (2) is larger than that of the sputtering block (1), and a plurality of mounting holes (3) are formed in the mounting ring (2) in an array mode.
9. The process for preparing an aluminum-chromium alloy target according to claim 1, wherein: the sheath (5) comprises two half blocks, and the sheath (5) is formed by splicing the two half blocks; a forming groove (4) matched with the shape of the alloy target is arranged in the sheath (5); the splicing surface of the left half block of the sheath (5) is provided with a matching bulge (7) protruding outwards, and the splicing surface of the right half block of the sheath (5) is provided with a matching groove (6) recessed inwards; the right end of the left half block of the sheath (5) is provided with a hinge block (10), the left end of the right half block of the sheath (5) is provided with a hinge frame (8) matched with the hinge block (10), an installation shaft (9) is fixedly welded in the hinge frame (8), a shaft hole matched with the installation shaft (9) is formed in a matching bulge (7), and the installation shaft (9) penetrates through the shaft hole to realize the hinge joint of the left half block and the right half block of the sheath (5); the other ends of the left half block and the right half block of the sheath (5) are respectively provided with a fixing block (11), and a fixing hole (12) for locking and fixing the sheath (5) is formed in the fixing block (11).
10. Use of a process according to any one of claims 1 to 9 for the preparation of an aluminium-chromium alloy target, wherein: the preparation process is used for producing and preparing the aluminum-titanium-chromium alloy target, the aluminum-titanium alloy target and the aluminum-chromium alloy target.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210394173.0A CN114769595A (en) | 2022-04-14 | 2022-04-14 | Preparation process and application of aluminum-chromium alloy target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210394173.0A CN114769595A (en) | 2022-04-14 | 2022-04-14 | Preparation process and application of aluminum-chromium alloy target |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114769595A true CN114769595A (en) | 2022-07-22 |
Family
ID=82429040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210394173.0A Pending CN114769595A (en) | 2022-04-14 | 2022-04-14 | Preparation process and application of aluminum-chromium alloy target |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114769595A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115341185A (en) * | 2022-10-18 | 2022-11-15 | 江苏集萃先进金属材料研究所有限公司 | Target material and manufacturing method thereof |
| CN116855902A (en) * | 2023-07-21 | 2023-10-10 | 苏州六九新材料科技有限公司 | Low-aluminum-content titanium-based target material and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513952A (en) * | 2013-09-30 | 2015-04-15 | 宁波江丰电子材料股份有限公司 | Manufacturing method of target material assembly and the target material assembly |
| CN208121188U (en) * | 2018-03-06 | 2018-11-20 | 南通安泰新材料科技有限公司 | A kind of rotation sial target assembly increased operation rate |
| CN208917291U (en) * | 2018-08-20 | 2019-05-31 | 山东格美钨钼材料股份有限公司 | A kind of structure of anti-gas-leak target jacket |
| US20190315041A1 (en) * | 2018-04-16 | 2019-10-17 | Sidel Participations | Molding Unit with Off-Center Neck Passage Opening |
| CN111197147A (en) * | 2020-02-20 | 2020-05-26 | 孙志颜 | Aluminum alloy and processing method thereof |
| CN113136554A (en) * | 2021-04-26 | 2021-07-20 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method thereof |
| CN113564544A (en) * | 2021-07-26 | 2021-10-29 | 宁波江丰电子材料股份有限公司 | Aluminum alloy target and preparation method thereof |
| CN214881799U (en) * | 2021-04-21 | 2021-11-26 | 漳州市合琦靶材科技有限公司 | High-performance high-quality alloy target material |
| CN113732284A (en) * | 2021-09-24 | 2021-12-03 | 河北宏靶科技有限公司 | Target material hot isostatic pressing forming method and equipment |
-
2022
- 2022-04-14 CN CN202210394173.0A patent/CN114769595A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513952A (en) * | 2013-09-30 | 2015-04-15 | 宁波江丰电子材料股份有限公司 | Manufacturing method of target material assembly and the target material assembly |
| CN208121188U (en) * | 2018-03-06 | 2018-11-20 | 南通安泰新材料科技有限公司 | A kind of rotation sial target assembly increased operation rate |
| US20190315041A1 (en) * | 2018-04-16 | 2019-10-17 | Sidel Participations | Molding Unit with Off-Center Neck Passage Opening |
| CN208917291U (en) * | 2018-08-20 | 2019-05-31 | 山东格美钨钼材料股份有限公司 | A kind of structure of anti-gas-leak target jacket |
| CN111197147A (en) * | 2020-02-20 | 2020-05-26 | 孙志颜 | Aluminum alloy and processing method thereof |
| CN214881799U (en) * | 2021-04-21 | 2021-11-26 | 漳州市合琦靶材科技有限公司 | High-performance high-quality alloy target material |
| CN113136554A (en) * | 2021-04-26 | 2021-07-20 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method thereof |
| CN113564544A (en) * | 2021-07-26 | 2021-10-29 | 宁波江丰电子材料股份有限公司 | Aluminum alloy target and preparation method thereof |
| CN113732284A (en) * | 2021-09-24 | 2021-12-03 | 河北宏靶科技有限公司 | Target material hot isostatic pressing forming method and equipment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115341185A (en) * | 2022-10-18 | 2022-11-15 | 江苏集萃先进金属材料研究所有限公司 | Target material and manufacturing method thereof |
| CN116855902A (en) * | 2023-07-21 | 2023-10-10 | 苏州六九新材料科技有限公司 | Low-aluminum-content titanium-based target material and preparation method thereof |
| CN116855902B (en) * | 2023-07-21 | 2024-04-16 | 苏州六九新材料科技有限公司 | Low-aluminum-content titanium-based target material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114769595A (en) | Preparation process and application of aluminum-chromium alloy target | |
| CN111958333A (en) | Polishing process of neodymium-aluminum target sputtering surface | |
| CN109972100B (en) | Preparation method of tubular chromium target | |
| CN113564544A (en) | Aluminum alloy target and preparation method thereof | |
| CN111945121A (en) | Tantalum-aluminum alloy sputtering target and preparation method thereof | |
| CN111270203A (en) | AlCrNbSiTiCN high-entropy alloy nano composite coating for die-casting die and preparation method thereof | |
| CN111593278B (en) | TiAl alloy near-isothermal forging method | |
| CN108555305B (en) | Ti2Method for preparing annular piece from AlNb alloy and TiAl powder | |
| CN110000391A (en) | A kind of preparation method of molybdenum tube | |
| CN108796304A (en) | A kind of γ-TiAl prealloys gas-atomized powder electrode bar and preparation method thereof | |
| EP0543353B1 (en) | Method for producing an inlet or exhaust valve for internal combustion engine | |
| CN112404426B (en) | Titanium-aluminum alloy die, preparation method of titanium-aluminum alloy outer sheath and method for performing spark plasma sintering by using titanium-aluminum alloy die | |
| CN114250444A (en) | Method for plasma-assisted chemical vapor deposition of high-purity tungsten sputtering target material | |
| CN112111714B (en) | Preparation method of tantalum-aluminum alloy sputtering target material | |
| CN112111719B (en) | Tungsten titanium silicon alloy sputtering target material and preparation method thereof | |
| CN112899624A (en) | Aluminum-silicon alloy sputtering target material and preparation method and application thereof | |
| CN113088909B (en) | Nickel-chromium alloy sputtering target material and hot-pressing preparation method thereof | |
| CN115255367B (en) | Nickel-aluminum alloy sputtering target material and hot pressing preparation method thereof | |
| WO2004005566A2 (en) | Method for making a composite product and in particular a heat sink | |
| CN1702191A (en) | Method for preparing alloy sheet | |
| CN111690925A (en) | Surface hardening and surface functionalization treatment process for titanium and titanium alloy | |
| CN112302830B (en) | Rhenium-iridium-carbon engine thrust chamber and integrated preparation method thereof | |
| CN114086130A (en) | Preparation method of tungsten-titanium alloy tube target | |
| CN104928539A (en) | Vanadium-aluminium-silicon ternary alloy target material and preparation method thereof | |
| CN113926856B (en) | Method for preparing dispersion-strengthened metal material in batch |
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 |