CN109554673A - A kind of cold spraying preparation process of aluminium rotary target material and products thereof - Google Patents
A kind of cold spraying preparation process of aluminium rotary target material and products thereof Download PDFInfo
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- CN109554673A CN109554673A CN201811300391.3A CN201811300391A CN109554673A CN 109554673 A CN109554673 A CN 109554673A CN 201811300391 A CN201811300391 A CN 201811300391A CN 109554673 A CN109554673 A CN 109554673A
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- cold spraying
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Coating By Spraying Or Casting (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a kind of cold spraying preparation processes of aluminium rotary target material, using aluminium powder as dusty spray raw material, carry out cold spraying using circulated helium cold spraying system；Cold spray process specifically: cold spraying chamber is evacuated to 0~500Pa, aluminium powder is sent into cold spraying system, using compressed helium as working gas, drives aluminium powder collision to be placed in matrix in cold spraying chamber, deposits to form dense coating in matrix surface；Undeposited aluminium powder enters filtration system in company with helium, and filtered helium returns to cold spraying system after entering gas pressurization system pressurization, collects undeposited aluminium powder and reuse after screening；In cold spray process, control cold spraying cavity indoor pressure maintains 5000~20000Pa.The bond strength of the cold spraying preparation process of aluminium rotary target material provided by the invention, simple process, aluminized coating and matrix is high, is not necessarily to transition zone.
Description
Technical field
The present invention relates to the preparation field of target more particularly to the cold spraying preparation processes and its production of a kind of aluminium rotary target material
Product.
Background technique
Rafifinal typically refers to the aluminium that purity (aluminium content) is greater than 99.8%, and rafifinal target is thin film transistor (TFT) (TFT)
The indispensable Coating Materials of industry, the plating of membrane of conducting layer on glass substrate.Currently, most of magnetron sputtering platings
The rafifinal target that producer uses belongs to flat target, its stock utilization is very low, only accounts for the material of gross mass 20% or so
It is utilized；Corresponding, the utilization rate of rafifinal rotary target then can achieve 75% or so.Moreover, if being come with KWh
The service life of target is measured, the service life of rotary target is about 5 times longer than the service life of flat target.In addition, recently as LCD screen
The continuous increase of size, according to rafifinal flat target, then the size of target must just increase with it.But if using rafifinal
Rotary target material, since the width of screen is only determined by the length of aluminum pipe, then the size of target is without adjustment.
Therefore, the use of rafifinal rotary target material, which has, simplifies magnetron sputtering membrane process, improves coating quality and big
Width reduces the advantages such as coating cost.
Currently, rafifinal rotary target material is generally using two methods of casting and cold spraying.
As Publication No. CN 107953084A Chinese patent literature in disclose a kind of manufacture of rafifinal rotary target material
Method, comprising: S1: selection rafifinal billet is target raw material, carries out hot piercing extrusion process to it, obtains rafifinal pipe；
S2: straightening processing is carried out to rafifinal pipe obtained by step S1；S3: the rafifinal pipe after step S2 straightening processing is moved back
Fire processing；S4: selection aluminium alloy is target tip materials, carries out surface hard oxidation processes to it, obtains aluminium alloy end；
S5: the rafifinal pipe after step S3 annealing is welded with aluminium alloy end obtained by step S4, obtains rafifinal conjunction
Gold target material.But the yield rate of casting is not high, while target crystalline grains tissue is coarseer, influences the quality of sputtered film.Due to
It is limited by casting size, target needs more sections of assembly splicings to cause gap to increase, and will affect plasma in coating process
Body uniformity consistency, and may cause the abnormal electric discharge in part, to reduce the uniformity and yields of film layer.
Cold spraying method is a kind of metal, ceramic spraying technique, different from traditional thermal spraying (including hypervelocity flame spray
Painting, plasma spraying, electric arc spraying etc.) technique, it does not need the metallic that will be sprayed fusing.Its principle utilized is: pressure
Contracting gas accelerates metallic to critical speed (supersonic speed), and after attacking directly to matrix surface physical deformation occurs for metallic, golden
Belong to particle hit it is flat in matrix surface and firm attachment.
Currently, cold spray process has been applied to the manufacturing field of metal rotation target, such as Publication No. CN 104831244A
Chinese patent literature in disclose a kind of aluminium tantalum rotary target material and method that controlled atmosphere cold spraying prepares aluminium tantalum rotary target material,
Method includes: that prepared sizes are 150~1000 mesh, and purity is not less than 99.99% aluminium tantalum powder；Under an inert atmosphere, it uses
Plasma-spray method sprays alloy transition layer on stainless steel base；In circulated inert gas protective atmosphere, cold spraying aluminium tantalum
Aluminium tantalum rotary target material is prepared on powder to the matrix for having very much alloy transition layer.
But currently, directly preparing the report of high-purity aluminized coating in substrate surface using cold spray process not yet.
Summary of the invention
The present invention provides a kind of cold spraying preparation process of aluminium rotary target material, simple process, the knots of aluminized coating and matrix
It is high to close intensity, is not necessarily to transition zone.
Specific technical solution is as follows:
A kind of cold spraying preparation process of aluminium rotary target material carries out cold spraying by dusty spray raw material of aluminium powder, described
Cold spraying uses circulated helium cold spraying system；
The circulated helium cold spraying system includes cold spraying system, cold spraying chamber, filtration system and gas boosting system
System；
The cold spraying, specifically:
Cold spraying chamber is evacuated to 0~500Pa, aluminium powder is sent into cold spraying system, using compressed helium as
Working gas drives aluminium powder collision to be placed in matrix in cold spraying chamber, to deposit to form dense coating in matrix surface；
Undeposited aluminium powder enters filtration system in company with helium, and filtered helium returns to after entering gas pressurization system pressurization
Cold spraying system collects undeposited aluminium powder, reuses after screening as powder reinforced phase；
In cold spray process, control cold spraying cavity indoor pressure maintains 5000~20000Pa.
Circulated helium cold spraying system introducing cold spray process is prepared aluminium rotary target material by the present invention, and helium is both work gas
Body is protective gas again, greatly improves target performance as working gas and production cost is greatly lowered, as protection gas
Body reduces target oxidation and impurity invasion.
It is found through experiment that being critical to when preparing aluminium target by cold spray process using the circulated helium cold spraying system
Control the indoor pressure of cold spraying chamber.If the pressure is maintained 5000~20000Pa, coating quality can be promoted.If pressure
Power is excessively high, and then particle speed reduces under same spraying conditions, coating quality deterioration.
In the circulated helium cold spraying system:
Cold spraying system is the equipment of dusty spray raw material, can specifically use Rafael nozzle.
Cold spraying chamber provides the environment of cold spraying for accommodating matrix；
Filtration system will guarantee passing through for helium for separating undeposited dusty spray raw material with helium,
Multi-stage screening method can specifically be used.
Helium after pressurization is passed through cold spraying system for pressurizeing to helium by gas pressurization system again, with
Realize recycling for helium.It specifically can be using centrifugation boosting method.
Preferably, the pressure of the working gas is 1~3MPa, and temperature is 200~400 DEG C.
Preferably, the dusty spray raw material is sent into cold spraying system by powder feeder, and powder feeding revolving speed is 3~10rpm.
Preferably, the outlet of the cold spraying system is apart from 20~30mm of matrix surface, if cold spraying system uses daraf(reciprocal of farad)
Your jet pipe, then the outlet of Rafael nozzle is 20~30mm apart from matrix surface, and the movement speed of Rafael nozzle is 60~
100mm/s。
It is further preferred:
In the cold spray process, control cold spraying cavity indoor pressure maintains 5000~10000Pa；
The pressure of the working gas is 2MPa, and temperature is 300 DEG C.
It is found through experiment that being had more using the aluminized coating of the surface of aluminum target material of the above-mentioned technological parameter preparation advanced optimized
High consistency.
The dusty spray raw material is aluminium powder, is selected from spherical powder, and partial size is 500 mesh~250 mesh.It is demonstrate,proved through test
Bright, the dusty spray raw material of the particle size range is the best particle size range of this technology route.
The aluminium powder is dried using preceding needs, is dried 1~3 hour such as in 80 DEG C of drying ovens.
Described matrix is selected from stainless steel tube, and the substrate of other types can also be selected according to customization.
The stainless steel tube is passing through surface sand-blasting process using preceding, specifically:
Sand-blast material is the Brown Alundum of 80 mesh partial sizes, and sandblasting angle is 30~45 °, and air compressor machine pressure is 0.8MPa.Roughening
The control of stainless steel roughness Ra is at 60~100 μm afterwards.
It is further preferred that stainless steel roughness Ra is controlled at 90~100 μm after roughening, the experiment proved that, the roughness
Under the conditions of, the bond strength of matrix and dusty spray raw material is optimal.
In spraying process, can control the revolving speed of stainless steel tube is 300rpm.
The invention also discloses the aluminium rotary target material prepared according to above-mentioned technique, the aluminium rotary target material, including matrix and
Aluminized coating, purity >=99.99% of the aluminized coating, consistency >=99%.
Compared with prior art, the beneficial effects of the present invention are:
The present invention carries out cold spraying using circulated helium cold spraying system and prepares aluminium target, the circulated helium cold spraying system
Include gas recycling, gas filtration, gas boosting, four part of cold spraying；Using the circulated helium cold spraying system, can guarantee not
The purity of raw material powder is deposited, non-deposited powder is greater than 300 mesh powder and reused, can be played the role of compacting, mentioned by screening
High target consistency.The present invention drives raw material powder in the solid state with 600~1000m/s or more using helium as working gas
Velocity collision matrix, the stroke speed of raw material powder is high, and the aluminized coating of preparation and the bond strength of matrix are high, is not necessarily to transition
Layer, and coating is fine and close, consistency >=99%, powder deposition efficiency is up to 99%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of circulated helium cold spraying system of the invention；
In figure, 1- cold spraying system, 2- cold spraying chamber, 3- filtration system, 4- gas pressurization system.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Circulated helium cold spraying system disclosed by the invention, including cold spraying system 1, cold spraying chamber 2, filtration system 3
And gas pressurization system 4.
Cold spraying system 1 is located in cold spraying chamber 2, and it is former which is equipped with working gas entrance, dusty spray
Expect entrance and outlet.Cold spraying system 1 in following embodiment is specifically using Rafael nozzle 11.
Stainless steel tube matrix is also placed in cold spraying chamber 2, the outlet of cold spraying chamber 2 is connected to filtration system 3, mistake
The outlet of filter system 3 is connected to gas pressurization system 4, and the outlet of gas pressurization system 4 and the work gas of cold spraying system 1
The connection of body entrance.
Filtration system 3 in following embodiment specifically uses multistage filter system, gas pressurization system 4 specifically using from
Heart booster.
The cold spraying course of work:
First cold spraying chamber 2 is vacuumized, dusty spray raw material is sent into Rafael nozzle 11 via powder feeder, utilizes pressure
Contracting helium drives dusty spray raw material to spray from the outlet of Rafael nozzle 11, in the solid state high velocity impact as working gas
The stainless steel tube matrix surface being placed in cold spraying chamber 2, so that deposition forms dense coating；In cold spray process, to tie up
The indoor pressure of cold spraying chamber is held under 5000~20000Pa range, undeposited dusty spray raw material entered in company with helium
Filter system 3, filtered helium enter gas pressurization system 4, are returned in cold spraying system 1 after being pressurized；Collection is not sunk
Long-pending dusty spray raw material continues to use as powder reinforced phase after screening.
Embodiment 1
1) prepared by stainless steel penstock:
Blanking: with 304 stainless steel tubes of sawing machine saw fetching measured length, the internal diameter of steel pipe is 125mm, outer diameter 133mm；
Che Guan: vehicle is distinguished by product drawing in stainless steel tube both ends and goes out groove, oblique angle etc.；
Surface sand-blasting roughening: stainless steel tube is passed through into sand-blasting machine for its surface sand-blasting process again；The sand-blast material is 80
The Brown Alundum of mesh partial size, sandblasting angle are 30 degree, and air compressor machine pressure is 0.8MPa, and stainless steel roughness (Ra), which controls, after roughening is
100 microns.
2) prepared by aluminium target:
Drying: being placed in aluminium powder (spherical powder, 500 mesh of partial size~250 mesh) in 80 DEG C of drying ovens and dry, the time 2
Hour；
Cold spraying: in 400~500Pa, powder feeding revolving speed is 6rpm, work gas for initial depression control in cold spraying chamber 2
Body pressure is 2MPa, and when powder feeding, it is 400 DEG C that working gas, which is heated to temperature, and the outlet of Rafael nozzle 11 is apart from stainless steel back
Pipe surface is 25mm, and it is 5000~10000Pa that pressure in cold spraying chamber 2 is controlled in cold spray process.
After tested, the aluminized coating consistency of embodiment preparation is 99.7%.
3) it is machined: after cold spraying gained target reaches client institute scale cun, molding rotary target material surface being used
Lathe is processed according to customer requirement, is cleaned, is dried again after completion of processing.
Embodiment 2
1) prepared by stainless steel penstock:
Blanking: with 304 stainless steel tubes of sawing machine saw fetching measured length, the internal diameter of steel pipe is 125mm, outer diameter 133mm；
Che Guan: vehicle is distinguished by product drawing in stainless steel tube both ends and goes out groove, oblique angle etc.；
Surface sand-blasting roughening: stainless steel tube is passed through into sand-blasting machine for its surface sand-blasting process again；The sand-blast material is 80
The Brown Alundum of mesh partial size, sandblasting angle are 45 degree, and air compressor machine pressure is 0.8MPa, and stainless steel roughness (Ra), which controls, after roughening is
60 microns；
2) prepared by aluminium target:
Drying: being placed in aluminium powder (spherical powder, 500 mesh of partial size~250 mesh) in 80 DEG C of drying ovens and dry, the time 3
Hour；
Cold spraying: in 400~500Pa, powder feeding revolving speed is 6rpm, work gas for initial depression control in cold spraying chamber 2
Body pressure is 3MPa, and it is 300 DEG C that working gas, which is heated to temperature, when powder feeding, and the outlet of Rafael nozzle is apart from stainless steel penstock table
Face is 25mm, and it is 10000~20000Pa that pressure in cold spraying chamber 2 is controlled in cold spray process.
After tested, the aluminized coating consistency of embodiment preparation is 99.5%.
3) it is machined: after cold spraying gained target reaches client institute scale cun, molding rotary target material surface being used
Lathe is processed according to customer requirement, is cleaned, is dried again after completion of processing.
Claims (8)
1. a kind of cold spraying preparation process of aluminium rotary target material carries out cold spraying, feature by dusty spray raw material of aluminium powder
It is, the cold spraying uses circulated helium cold spraying system；
The circulated helium cold spraying system includes cold spraying system, cold spraying chamber, filtration system and gas pressurization system；
The cold spraying, specifically:
Cold spraying chamber is evacuated to 0~500Pa, aluminium powder is sent into cold spraying system, using compressed helium as work
Gas drives aluminium powder collision to be placed in matrix in cold spraying chamber, to deposit to form dense coating in matrix surface；It does not sink
Long-pending aluminium powder enters filtration system in company with helium, and filtered helium returns to cold spray after entering gas pressurization system pressurization
Painting system collects undeposited aluminium powder, reuses after screening as powder reinforced phase；
In cold spray process, control cold spraying cavity indoor pressure maintains 5000~20000Pa.
2. the cold spraying preparation process of aluminium rotary target material according to claim 1, which is characterized in that the working gas
Pressure is 1~3MPa, and temperature is 200~400 DEG C.
3. the cold spraying preparation process of aluminium rotary target material according to claim 1, which is characterized in that the aluminium powder is selected from
Spherical powder, partial size are 500 mesh~250 mesh.
4. the cold spraying preparation process of aluminium rotary target material according to claim 1, which is characterized in that the aluminium powder passes through
Powder feeder is sent into cold spraying system, and powder feeding revolving speed is 3~10rpm.
5. the cold spraying preparation process of aluminium rotary target material according to claim 1, which is characterized in that the cold spraying system
Outlet apart from 20~30mm of matrix surface.
6. the cold spraying preparation process of aluminium rotary target material according to claim 1, which is characterized in that described matrix is selected from not
Become rusty steel pipe；
The stainless steel tube is passing through surface sand-blasting process using preceding, specifically:
Sand-blast material is the Brown Alundum of 80 mesh partial sizes, and sandblasting angle is 30~45 °, and air compressor machine pressure is 0.8MPa, after roughening not
The control of steel roughness Ra become rusty at 60~100 μm.
7. the cold spraying preparation process of aluminium rotary target material according to claim 1, which is characterized in that undeposited aluminium powder
End, after screening, the aluminium powder that collection cut size is greater than 300 mesh is reused as powder reinforced phase.
8. a kind of aluminium rotary target material of the technique preparation any according to claim 1~7, which is characterized in that including matrix
And aluminized coating, purity >=99.99% of the aluminized coating, consistency >=99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811300391.3A CN109554673A (en) | 2018-11-02 | 2018-11-02 | A kind of cold spraying preparation process of aluminium rotary target material and products thereof |
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| CN201811300391.3A CN109554673A (en) | 2018-11-02 | 2018-11-02 | A kind of cold spraying preparation process of aluminium rotary target material and products thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653971A (en) * | 2022-03-30 | 2022-06-24 | 广东省科学院新材料研究所 | Hydrogen-powered metal solid deposition device and method |
| CN115584497A (en) * | 2022-10-31 | 2023-01-10 | 上海交通大学 | Cold spraying material increase and decrease integrated equipment with recyclable powder and gas |
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| CN115584497A (en) * | 2022-10-31 | 2023-01-10 | 上海交通大学 | Cold spraying material increase and decrease integrated equipment with recyclable powder and gas |
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Application publication date: 20190402 |