CN106498350A - The preparation method of sial sputtering target material - Google Patents
The preparation method of sial sputtering target material Download PDFInfo
- Publication number
- CN106498350A CN106498350A CN201610891073.3A CN201610891073A CN106498350A CN 106498350 A CN106498350 A CN 106498350A CN 201610891073 A CN201610891073 A CN 201610891073A CN 106498350 A CN106498350 A CN 106498350A
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- base tube
- target
- sial
- spraying
- powder
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of high density, low oxygen content, the preparation method of non-fragile sial sputtering target material, comprise the steps：Target base tube prepares：From and check the rustless steel base tube of required model；Base tube surface preparation：Base tube entrance base tube pre-processing device is carried out sandblasting roughening, uses ni-al alloyed wire, arc spraying sprays bottoming binder courses, obtain the target base tube for preparing spraying；Raw material prepares：Weigh content：99.9% 99.95%, oxygen content≤1000ppm, particle diameter：The silica flour 50kg of 45 150um；Weigh content：99.9% 99.95%, oxygen content≤1500ppm, particle diameter：The high pure spherical aluminium powder 6.6kg of 45 100um；Mixed powder：By mixed for 2 kinds of raw material input V-types of gained powder machine, mix 56 hours；Dry：The sial powder raw material of mix homogeneously is placed in drying oven, is dried 23 hours, temperature 60 C.
Description
Technical field
A kind of the present invention relates to sputter coating Material Field, more particularly to preparation method of sial target.
Background technology
In recent years, physical vapour deposition (PVD) sputter coating process is growing, and the quality of target quality directly influences film
Quality, as silicon aluminum alloy material possesses good superhard, wear-resisting, against corrosion, the feature that closure is good, sial target is energy-conservation glass
Indispensable film material in glass, decoration panel sputter coating process, is widely used.Limitation due to production technology
Property, the sial target that current China uses, overall have relative density not high enough（≤95%）, hole is more, oxygen content is high, use
In easy embrittlement defect.In sputter procedure, as target density is not high enough, material is of a relatively loose, around target high-speed motion
Charged ion bombardment target material surface when, target atom group not of uniform size can be fired out and be deposited on substrate, film layer is just not enough
Fine and close smooth, have concavo-convex, meanwhile, sputtering target material surface instantaneous high-temperature easily makes discrete particles group dress drop, and pollutes glass surface,
Affect coating quality.As target internal void is more, during spatter film forming, the gas that target internal void is present can be quick-fried suddenly
Broken cause microgranule to splash, pollution film layer surface makes that film is fine and close, rough surface, and defect increases.In target, oxygen content is high, causes
Target electric conductivity in sputter procedure is deteriorated, and have impact on electric discharge build-up of luminance, and sputter rate is deteriorated, simultaneously because oxygen content is high, is splashing
During penetrating, the oxygen evolution in target uprises the oxygen concentration in vacuum chamber in sputtering chamber vacuum chamber, and sputtered out will
The target atom group of film forming is oxidized, partly changes the chemical attribute of target material, have impact on the quality of film.Target is being used
Middle embrittlement mainly has several reasons, and one is that density is relatively low, internal bond strength is inadequate；Two is material segregation, skewness；Three is target
There is stress inside material, factors above is such as heated, collides i.e. generation embrittlement when external force factor is run into.
Content of the invention
The technical problem to be solved is：A kind of high density, low oxygen content, the sputtering of non-fragile sial are provided
The preparation method of target.
In order to solve above-mentioned technical problem, the technical scheme is that：The preparation method of sial sputtering target material, including as
Lower step：Target base tube prepares：From and check the rustless steel base tube of required model；Base tube surface preparation：Base tube is entered
Base tube pre-processing device carries out sandblasting roughening, uses ni-al alloyed wire, and arc spraying sprays bottoming binder courses, obtains preparing spray
The target base tube of painting；Raw material prepares：Weigh content：99.9%-99.95%, oxygen content≤1000ppm, particle diameter：45-150um's
Silica flour 50kg；Weigh content：99.9%-99.95%, oxygen content≤1500ppm, particle diameter：The high pure spherical aluminium powder of 45-100um
6.6kg；Mixed powder：By mixed for 2 kinds of raw material input V-types of gained powder machine, mix 5-6 hours；Dry：The aluminum silicon powder of mix homogeneously is former
Material is placed in drying oven, dries 2-3 hours, temperature 60 C；Preheating：Target base tube is placed in the spraying storehouse of sealing, by target pipe
Inside is connected with circulating water device, and starts warmer, target pipe is preheated to 80 DEG C and keeps constant temperature；Vacuum plasma sprays
Apply：Using high-power Supersonic Plasma Spraying rifle, gained sial dusty material is heated to melt for thermal source using plasma
Melt or semi-molten state, the target base tube surface for preparing is sprayed to high speed flame stream, form fine and close silicon-aluminium alloy target material and apply
Layer, in spraying process, is passed through nitrogen, and is in barotropic state in the continuous storehouse toward spraying；Spray voltage 95-100V, spraying electricity
Stream 550-600A, argon flow amount 1500-2500L/h, 10000-15000 DEG C of flame passes temperature, flame flow velocity degree 150m/s,
Make sial powder melt in moment, and target base tube surface is sprayed to by high speed flame stream is very fast, form sedimentary；Hydrogen stream 600-
1500L/h, nitrogen flow 3000-4000L/h, hydrogen is used as Ar ion mixing gas；Cooling：After the completion of spraying coating process, close and supply powder
System, closes paint finishing, starts gradient cooling system, i.e., extend 2-3 times of duration than Temperature fall, be down to room temperature；Machinery adds
Work：After target export after the completion of cooling, profile machining is carried out, packaging is cleaned after processing and obtains sial sputtering target
Material.
It is an advantage of the invention that：The preparation method of above-mentioned sial sputtering target material, has improved sial target key
Quality index, greatly improves properties of product, has great impetus, the impurity in the present invention to the development of plated film industry
Summation≤1000ppm, oxygen content≤1500ppm, crystal grain≤50 μm of relative density >=97% target, close due to sial target
Degree is improved, and oxygen content is controlled, and internal stress is released, and crystal grain is refined, its sputter rate faster, use
Life-span is longer, will not embrittlement, the quality of gained thin film is higher.
Specific embodiment
Below by the particular content that specific embodiment describes in detail the present invention.
The preparation method of sial sputtering target material, comprises the steps：Target base tube prepares：From and check required model
Rustless steel base tube；Base tube surface preparation：Base tube entrance base tube pre-processing device is carried out sandblasting roughening, uses nickel alumin(i)um alloy
Silk, arc spraying spray bottoming binder courses, obtain the target base tube for preparing spraying；Raw material prepares：Weigh content：99.9%-
99.95%th, oxygen content≤1000ppm, particle diameter：The silica flour 50kg of 45-150um；Weigh content：99.9%-99.95%, oxygen content
≤ 1500ppm, particle diameter：The high pure spherical aluminium powder 6.6kg of 45-100um；Mixed powder：By mixed for 2 kinds of raw material input V-types of gained powder
Machine, mixes 5-6 hours；Dry：The sial powder raw material of mix homogeneously is placed in drying oven, 2-3 hours, temperature 60 C is dried；
Preheating：Target base tube is placed in the spraying storehouse of sealing, will be connected with circulating water device inside target pipe, and started warmer,
Target pipe is preheated to 80 DEG C and keeps constant temperature so as to the temperature difference is reduced with by the melted material for being sprayed at its surface, blending is more preferable；
Vacuum plasma spray coating：Using high-power Supersonic Plasma Spraying rifle, the use of plasma is thermal source by gained sial powder
Material is heated to melting or semi-molten state, sprays to the target base tube surface for preparing with high speed flame stream, forms fine and close silicon
Aluminium alloy target coating, in spraying process, is passed through nitrogen in the continuous storehouse toward spraying, and is in barotropic state, to ensure target
Spraying overall process all in inert gas shielding state in, whole spraying process not with air contact, to ensure the hypoxia of target
Property；Spray voltage 95-100V, spraying current 550-600A, argon flow amount 1500-2500L/h, flame passes temperature
10000-15000 DEG C, flame flow velocity degree 150m/s, make sial powder melt in moment, and are sprayed to target by high speed flame stream is very fast
Base tube surface, forms sedimentary, due to raw materials melt thoroughly, sprays very fast strong, the densification of target material deposition layer, uniform, hole pole
Little, structural capacity is strong；Hydrogen stream 600-1500L/h, nitrogen flow 3000-4000L/h, hydrogen as Ar ion mixing gas, on the one hand
Plasma gun power can be improved, flame body temperature and flame flow velocity degree is improved, the reproducibility of raw material on the other hand, can be promoted, it is ensured that
Original physicochemical characteristicses of raw material；Cooling：After the completion of spraying coating process, powder-supply system is closed, close paint finishing, start gradient drop
Warm system, i.e., extend 2-3 times of duration than Temperature fall, be down to room temperature, allows the internal stress of target to discharge and more completely, does not answer
Power is gathered；Machining：After target export after the completion of cooling, profile machining is carried out, packaging is cleaned after processing i.e.
Obtain sial sputtering target material.
Claims (1)
1. the preparation method of sial sputtering target material, it is characterised in that：Comprise the steps：Target base tube prepares：From and check
The rustless steel base tube of required model；Base tube surface preparation：Base tube entrance base tube pre-processing device is carried out sandblasting roughening, use
Ni-al alloyed wire, arc spraying spray bottoming binder courses, obtain the target base tube for preparing spraying；Raw material prepares：Weigh content：
99.9%-99.95%, oxygen content≤1000ppm, particle diameter：The silica flour 50kg of 45-150um；Weigh content：99.9%-99.95%、
Oxygen content≤1500ppm, particle diameter：The high pure spherical aluminium powder 6.6kg of 45-100um；Mixed powder：2 kinds of raw material input V-types by gained
Mixed powder machine, mixes 5-6 hours；Dry：The sial powder raw material of mix homogeneously is placed in drying oven, 2-3 hours, temperature 60 is dried
℃ ；Preheating：Target base tube is placed in the spraying storehouse of sealing, will be connected with circulating water device inside target pipe, and started heating
Target pipe is preheated to 80 DEG C and keeps constant temperature by device；Vacuum plasma spray coating：Using high-power Supersonic Plasma Spraying rifle, make
Be that gained sial dusty material is heated to melting or semi-molten state by thermal source with plasma, preparation is sprayed to high speed flame stream
Good target base tube surface, forms fine and close silicon-aluminium alloy target material coating, in spraying process, is passed through in the continuous storehouse toward spraying
Nitrogen, and be in barotropic state；Spray voltage 95-100V, spraying current 550-600A, argon flow amount 1500-2500L/h, etc. from
Sub- flame body temperature 10000-15000 DEG C, flame flow velocity degree 150m/s, make sial powder melt in moment, and very fast by high speed flame stream
Target base tube surface is sprayed to, sedimentary is formed；Hydrogen stream 600-1500L/h, nitrogen flow 3000-4000L/h, hydrogen conduct
Ar ion mixing gas；Cooling：After the completion of spraying coating process, powder-supply system is closed, close paint finishing, start gradient cooling system, i.e.,
Extend 2-3 times of duration than Temperature fall, be down to room temperature；Machining：After target export after the completion of cooling, profile machinery is carried out
Processing, is cleaned packaging and obtains sial sputtering target material after processing.
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| CN201610891073.3A CN106498350A (en) | 2016-10-13 | 2016-10-13 | The preparation method of sial sputtering target material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707870A (en) * | 2018-05-24 | 2018-10-26 | 宁波森利电子材料有限公司 | The preparation method of the sial rotary target material of high-compactness |
| CN108728786A (en) * | 2018-04-11 | 2018-11-02 | 中国人民解放军陆军装甲兵学院 | A method of preparing silumin coating |
| CN108772567A (en) * | 2018-06-29 | 2018-11-09 | 米亚索乐装备集成（福建）有限公司 | A kind of alloy material for CIG target prime coats, CIG targets and preparation method thereof |
| CN110133783A (en) * | 2019-05-17 | 2019-08-16 | 东莞市微科光电科技有限公司 | A kind of infrared narrow band filter manufacturing method |
| CN111041432A (en) * | 2019-11-26 | 2020-04-21 | 广州市尤特新材料有限公司 | Rotary zirconia target material and preparation method thereof |
| CN113233786A (en) * | 2021-06-28 | 2021-08-10 | 重庆市渝大节能玻璃有限公司 | Preparation process of colored glass |
| CN113502456A (en) * | 2021-07-22 | 2021-10-15 | 法柯特科技（江苏）有限公司 | Preparation process of silicon-boron-carbon sputtering target material |
| CN113862621A (en) * | 2021-09-17 | 2021-12-31 | 芜湖映日科技股份有限公司 | Preparation method of rotary silicon-chromium target |
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| CN101403088A (en) * | 2008-11-13 | 2009-04-08 | 中南大学 | Silicon-aluminium alloy target material with high silicon content for sputtering and coating film, and method of producing the same |
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Patent Citations (5)
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| CN101403088A (en) * | 2008-11-13 | 2009-04-08 | 中南大学 | Silicon-aluminium alloy target material with high silicon content for sputtering and coating film, and method of producing the same |
| CN102286717A (en) * | 2011-09-01 | 2011-12-21 | 基迈克材料科技（苏州）有限公司 | Cylindrical large-area film coating target prepared through plasma spray coating and method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728786A (en) * | 2018-04-11 | 2018-11-02 | 中国人民解放军陆军装甲兵学院 | A method of preparing silumin coating |
| CN108707870A (en) * | 2018-05-24 | 2018-10-26 | 宁波森利电子材料有限公司 | The preparation method of the sial rotary target material of high-compactness |
| CN108772567A (en) * | 2018-06-29 | 2018-11-09 | 米亚索乐装备集成（福建）有限公司 | A kind of alloy material for CIG target prime coats, CIG targets and preparation method thereof |
| CN110133783A (en) * | 2019-05-17 | 2019-08-16 | 东莞市微科光电科技有限公司 | A kind of infrared narrow band filter manufacturing method |
| CN110133783B (en) * | 2019-05-17 | 2021-08-31 | 东莞市微科光电科技有限公司 | Manufacturing method of infrared narrow-band filter |
| CN111041432A (en) * | 2019-11-26 | 2020-04-21 | 广州市尤特新材料有限公司 | Rotary zirconia target material and preparation method thereof |
| CN113233786A (en) * | 2021-06-28 | 2021-08-10 | 重庆市渝大节能玻璃有限公司 | Preparation process of colored glass |
| CN113502456A (en) * | 2021-07-22 | 2021-10-15 | 法柯特科技（江苏）有限公司 | Preparation process of silicon-boron-carbon sputtering target material |
| CN113862621A (en) * | 2021-09-17 | 2021-12-31 | 芜湖映日科技股份有限公司 | Preparation method of rotary silicon-chromium target |
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