CN108707870A - The preparation method of the sial rotary target material of high-compactness - Google Patents
The preparation method of the sial rotary target material of high-compactness Download PDFInfo
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- CN108707870A CN108707870A CN201810509361.7A CN201810509361A CN108707870A CN 108707870 A CN108707870 A CN 108707870A CN 201810509361 A CN201810509361 A CN 201810509361A CN 108707870 A CN108707870 A CN 108707870A
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- target
- sial
- penstock
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- target material
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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
- 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
- C23C4/067—Metallic material containing free particles of non-metal elements, e.g. carbon, silicon, boron, phosphorus or arsenic
-
- 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
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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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)
- Coating By Spraying Or Casting (AREA)
Abstract
The invention discloses a kind of preparation methods of the sial rotary target material of high-compactness, including prepare dusty spray, pretreatment target penstock, prepare in target penstock to target penstock spraying prime coat, with plasma spray coating process sial target.Wherein, the method for preparing dusty spray is：By percentage to the quality, after the silica flour of 90%-92% being mixed with the aluminium powder of 8%-10%, powder is uniformly mixed in V-type mixes powder machine 4-6 hours, then dried 4-6 hours in 90-110 ° of drying box.It is an advantage of the invention that：Simple for process, prepared target quality is preferable.
Description
Technical field
The present invention relates to target technical fields, more particularly, to a kind of preparation side of the sial rotary target material of high-compactness
Method.
Background technology
Magnetron sputtering technique is a kind of advanced high-quality thin film deposition approach.Its working principle is that：Electronics is in electric field
Effect is lower to be accelerated to collide with sputter gas atom during flying to substrate, ionizes out a large amount of cation and electronics.Electricity
Son flies to substrate, and cation accelerates to bombard target under the action of electric field, sputters a large amount of target atom, the target being in neutrality
Atom (or molecule), which is deposited on, ultimately forms required film on substrate.
Silicon (Si) based sputtering target material is with the fastest developing speed in numerous sputtering target materials and applies a kind of wider target.Si is
A kind of traditional semi-conducting material, in recent years since the development that magnetron sputtering prepares thin film technique makes it be obtained in many fields
New application.The silica-base film of magnetron sputtering deposition has been applied in touch sensor, building energy conservation Low-E glass at present,
And the fields such as car coated glass.
Magnetron sputtering is generally made up of plasma spray coating process with sial target, but obtained target consistency is relatively low,
Relative density only has 90% or so.Easily there is the defects of dross, picking in sputtering process in the target of low-density, influences plated film production
The quality and production stability of product.Application publication number is the Chinese invention patent application of CN106498350A：Sial sputtering target material
Preparation method, disclose a kind of by vacuum atm plasma spraying technology, relative density be made up to 97% sial target.
But do not state that it actually prepares the density of target with this method in the patent.And vacuum plasma spray coating is compared with air etc.
Plasma spray, increase penstock preheat, vacuumize, be filled with the series of steps such as inert protective gas, complex process and cost compared with
It is high.
Invention content
The object of the present invention is to provide a kind of preparation methods of the sial rotary target material of high-compactness, it has technique letter
Feature single, prepared target quality is preferable.
The technical solution adopted in the present invention is：
The preparation method of the sial rotary target material of high-compactness, includes the following steps：
(1) dusty spray is prepared；
(2) target penstock is pre-processed；
(3) prime coat is sprayed to target penstock；
(4) sial target is prepared in target penstock with plasma spray coating process.
In the step (1), the method for preparing dusty spray is：By percentage to the quality, by the silica flour of 90%-92% with
After the aluminium powder mixing of 8%-10%, powder is uniformly mixed in V-type mixes powder machine 4-6 hours, then dried in 90-110 ° of drying box
It is 4-6 hours dry.
The silica flour purity is not less than 99.9%, in the silica flour, by percentage to the quality, the grain of the silica flour of 20%-50%
Degree is 125-160 μm, remaining silicon particle size is 45-125 μm.
The aluminium powder purity is 75-100 μm not less than 99.9%, granularity.
In the step (2), the method for pretreatment target penstock is：Ultrasonic cleaning, then sandblasting are roughened.
In the step (3), it is to target penstock spraying prime coat：Using electric arc spraying in target penstock surface spraying
Nickel alumin(i)um alloy.
In the step (4), with plasma spray coating process during preparing sial target in target penstock, work is sprayed
The speed of mainshaft of dress is 200-240r/min, and the spray distance control between spray gun and penstock is 100-130mm, the mobile speed of spray gun
Degree is 2000-2400mm/min.
In the step (4), with plasma spray coating process during preparing sial target in target penstock, target is controlled
Material surface temperature is no more than 90 DEG C.
The invention has the advantages that compared with the prior art,：Simple for process, prepared target quality is preferable.This hair
Target material structure prepared by the preparation method of the sial rotary target material of bright high-compactness is fine and close, ingredient uniformly, good conductivity, nothing
Crackle, spraying length and diameter is unrestricted, and thickness is not less than 93% up to 13mm, relative density, and provided by the invention
Preparation method, production process is simple and convenient, and cost is relatively low.
Specific implementation mode
Embodiment 1
The preparation method of the sial rotary target material of high-compactness, specially in outer diameter 133mm, the target of length 850mm is carried on the back
Guan Shang, sial target of the spraying not less than 4mm thickness.Include the following steps：
(1) dusty spray is prepared；
(2) target penstock is pre-processed；
(3) prime coat is sprayed to target penstock；
(4) sial target is prepared in target penstock with plasma spray coating process.
Wherein：
In step (1), the method for preparing dusty spray is：By percentage to the quality, by 90% silica flour and 10% aluminium
After powder mixing, powder is uniformly mixed in V-type mixes powder machine 4 hours, then dried 4 hours in 90 ° of drying box.
Meanwhile the silica flour purity of use is not less than 99.9%.In the silica flour, by percentage to the quality, 20% silica flour
Average particle size is 125 μm, and the average particle size of remaining silica flour is 45 μm.Aluminium powder purity is 75 μm not less than 99.9%, average particle size.
In step (2), the method for pretreatment target penstock is：By sial target in supersonic wave cleaning machine ultrasonic cleaning
40 minutes, then sandblasting was roughened.
In step (3), it is to target penstock spraying prime coat：Using electric arc spraying in target penstock surface spraying thickness
For 0.1mm nickel alumin(i)um alloys.The specific process parameter of electric arc spraying can be shown in Table 1：
The technological parameter of 1 electric arc spraying prime coat of table
| Technological parameter | Voltage | Electric current | Silk material diameter | Wire feed rate | Spray pressure |
| Parameter value | 40V | 350A | 2.5mm | 130mm/s | 0.5MPa |
In step (4), with plasma spray coating process during preparing sial target in target penstock, spraying frock
The speed of mainshaft is 200r/min, and the spray distance control between spray gun and penstock is 100mm, and the movement speed of spray gun is 2000mm/
min。
In step (4), with plasma spray coating process during preparing sial target in target penstock, target table is controlled
Face temperature is no more than 90 DEG C.For example, integrated use water cooling tube and compressed gas cooling spraying target.
Sial rotary target material prepared by the present embodiment 1 is black, thickness 4.2mm, with Archimedes's drainage detection density
For 2.201g/cm3, relative density 93.3%, resistivity is 11.7m Ω .cm, illustrates that its compact structure, electric conductivity are preferable, and
Detect flawless.Meanwhile compared with the modes such as vacuum plasma spray coating, the preparation method of the present embodiment without being vacuumized,
Protective gas is filled, to which cost is relatively low, production process is simple and convenient.The present embodiment is introduced into carries out mixed powder in V-type machine
The step of, it is ensured that product composition is more uniform.
Embodiment 2
The preparation method of the sial rotary target material of high-compactness, specially in outer diameter 133mm, the target of length 3191mm is carried on the back
Guan Shang, sial target of the spraying not less than 9mm thickness.Include the following steps：
(1) dusty spray is prepared；
(2) target penstock is pre-processed；
(3) prime coat is sprayed to target penstock；
(4) sial target is prepared in target penstock with plasma spray coating process.
Wherein：
In step (1), the method for preparing dusty spray is：By percentage to the quality, by 91% silica flour and 9% aluminium powder
After mixing, powder is uniformly mixed in V-type mixes powder machine 5 hours, then dried 5 hours in 100 ° of drying box.
Meanwhile the silica flour purity of use is not less than 99.9%.In the silica flour, by percentage to the quality, 35% silica flour
Average particle size is 135 μm, remaining silica flour average particle size is 80 μm.Aluminium powder purity is 80 μm not less than 99.9%, average particle size.
In step (2), the method for pretreatment target penstock is：By sial target in supersonic wave cleaning machine ultrasonic cleaning
30 minutes, then sandblasting was roughened.
In step (3), it is to target penstock spraying prime coat：Using electric arc spraying in target penstock surface spraying thickness
For 0.2mm nickel alumin(i)um alloys.The specific process parameter of electric arc spraying can be shown in Table 2：
The technological parameter of 2 electric arc spraying prime coat of table
| Technological parameter | Voltage | Electric current | Silk material diameter | Wire feed rate | Spray pressure |
| Parameter value | 40V | 370A | 2.5mm | 150mm/s | 0.5MPa |
In step (4), with plasma spray coating process during preparing sial target in target penstock, spraying frock
The speed of mainshaft is 230r/min, and the movement speed of spray distance 110mm, spray gun are 2200mm/min,
In step (4), with plasma spray coating process during preparing sial target in target penstock, target table is controlled
Face temperature is no more than 90 DEG C.For example, integrated use water cooling tube and compressed gas cooling spraying target.
Sial rotary target material prepared by the present embodiment 2 is black, thickness 9.1mm, with Archimedes's drainage detection density
For 2.209g/cm3, relative density 93.6%, resistivity is 11.2m Ω .cm, illustrates that its compact structure, electric conductivity are preferable, and
Detect flawless.Meanwhile compared with the modes such as vacuum plasma spray coating, the preparation method of the present embodiment without being vacuumized,
Protective gas is filled, to which cost is relatively low, production process is simple and convenient.The present embodiment is introduced into carries out mixed powder in V-type machine
The step of, it is ensured that product composition is more uniform.
Embodiment 3
The preparation method of the sial rotary target material of high-compactness, specially in outer diameter 133mm, the target of length 850mm is carried on the back
Guan Shang, sial target of the spraying not less than 4mm thickness.Include the following steps：
(1) dusty spray is prepared；
(2) target penstock is pre-processed；
(3) prime coat is sprayed to target penstock；
(4) sial target is prepared in target penstock with plasma spray coating process.
Wherein：
In step (1), the method for preparing dusty spray is：By percentage to the quality, by 92% silica flour and 8% aluminium powder
After mixing, powder is uniformly mixed in V-type mixes powder machine 6 hours, then dried 6 hours in 110 ° of drying box.
Meanwhile the silica flour purity of use is not less than 99.9%.In the silica flour, by percentage to the quality, 40% silica flour
Average particle size is 150 μm, remaining silica flour average particle size is 125 μm.Aluminium powder purity is 100 μm not less than 99.9%, average particle size.
In step (2), the method for pretreatment target penstock is：By sial target in supersonic wave cleaning machine ultrasonic cleaning
50 minutes, then sandblasting was roughened.
In step (3), it is to target penstock spraying prime coat：Using electric arc spraying in target penstock surface spraying thickness
For 0.2mm nickel alumin(i)um alloys.The specific process parameter of electric arc spraying can be shown in Table 3：
The technological parameter of 32 electric arc spraying prime coat of table
| Technological parameter | Voltage | Electric current | Silk material diameter | Wire feed rate | Spray pressure |
| Parameter value | 45V | 350A | 2.5mm | 150mm/s | 0.5MPa |
In step (4), with plasma spray coating process during preparing sial target in target penstock, spraying frock
The speed of mainshaft is 240r/min, and the spray distance control between spray gun and penstock is 130mm, and the movement speed of spray gun is 2400mm/
min。
In step (4), with plasma spray coating process during preparing sial target in target penstock, target table is controlled
Face temperature is no more than 90 DEG C.For example, integrated use water cooling tube and compressed gas cooling spraying target.
Sial rotary target material prepared by the present embodiment 3 is black, and thickness 13mm is with Archimedes's drainage detection density
2.197g/cm3, relative density 93.07%, resistivity are 9m Ω .cm, illustrate that its compact structure, electric conductivity are preferable, and are detected
Flawless.Meanwhile compared with the modes such as vacuum plasma spray coating, the preparation method of the present embodiment is without being vacuumized, filling guarantor
Shield gas and etc., to which cost is relatively low, production process is simple and convenient.The present embodiment is introduced into the step that mixed powder is carried out in V-type machine
Suddenly, it is ensured that product composition is more uniform.
In conclusion the preparation method of the sial rotary target material of the high-compactness of the present invention mainly passes through silica flour different-grain diameter
Changes of contents, form highdensity effect.That is, under identical plasma spraying power, the powder thawing of fine grain is more filled
Point, it is easy to be accelerated to higher speed, obtained spray-on coating density is high, but coating thermal stress is big, easy to crack, does not have to generally
In spraying relatively thick coating；The powder thawing of coarse grain diameter is insufficient, and dusty spray speed is smaller, and gained coating porosity is high, density
It is low, but coating thermal stress is smaller, it is not easy to crack, it can be used for spraying relatively thick coating.The content that the present invention passes through silica flour different-grain diameter
Variation, under the premise of not improving target tearing tendency, improves target density.The relative density by silicon target is embodied in by 90%
It improves to 93% or more.Due to the raising of density, the abnormal appearance such as reduction target dross occurs, beats arc in use,
Improve coating quality and efficiency.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the scope of the invention, every utilization
Equivalent process transformation made by present specification is applied directly or indirectly in other relevant technical fields, same
Reason is included within the scope of the present invention.
Claims (8)
1. the preparation method of the sial rotary target material of high-compactness, includes the following steps：
(1) dusty spray is prepared；
(2) target penstock is pre-processed；
(3) prime coat is sprayed to target penstock；
(4) sial target is prepared in target penstock with plasma spray coating process.
2. the preparation method of the sial rotary target material of high-compactness according to claim 1, it is characterised in that：The step
(1) in, the method for preparing dusty spray is：By percentage to the quality, the aluminium powder of the silica flour of 90%-92% and 8%-10% is mixed
After conjunction, powder is uniformly mixed in V-type mixes powder machine 4-6 hours, then dried 4-6 hours in 90-110 ° of drying box.
3. the preparation method of the sial rotary target material of high-compactness according to claim 2, it is characterised in that：The silica flour
Purity is not less than 99.9%, and in the silica flour, by percentage to the quality, the granularity of the silica flour of 20%-50% is 125-160 μm,
Remaining silicon particle size is 45-125 μm.
4. the preparation method of the sial rotary target material of high-compactness according to claim 2, it is characterised in that：The aluminium powder
Purity is 75-100 μm not less than 99.9%, granularity.
5. the preparation method of the sial rotary target material of high-compactness according to claim 1, it is characterised in that：The step
(2) in, the method for pretreatment target penstock is：Ultrasonic cleaning, then sandblasting are roughened.
6. the preparation method of the sial rotary target material of high-compactness according to claim 1, it is characterised in that：The step
(3) in, it is to target penstock spraying prime coat：Using electric arc spraying in target penstock surface spraying nickel alumin(i)um alloy.
7. the preparation method of the sial rotary target material of high-compactness according to claim 1, it is characterised in that：The step
(4) in, with plasma spray coating process during preparing sial target in target penstock, the speed of mainshaft of spraying frock is
200-240r/min, the spray distance control between spray gun and penstock are 100-130mm, and the movement speed of spray gun is 2000-
2400mm/min。
8. the preparation method of the sial rotary target material of high-compactness according to claim 1, it is characterised in that：The step
(4) in, with plasma spray coating process during preparing sial target in target penstock, control target material surface temperature is no more than
90℃。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881162A (en) * | 2018-11-29 | 2019-06-14 | 芮瑛 | A kind of sputtering target material preparation process based on plasma spraying technology |
| CN112899628A (en) * | 2021-01-18 | 2021-06-04 | 福建阿石创新材料股份有限公司 | Rotary silicon target material capable of being uniformly sputtered and preparation method thereof |
| 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881162A (en) * | 2018-11-29 | 2019-06-14 | 芮瑛 | A kind of sputtering target material preparation process based on plasma spraying technology |
| CN112899628A (en) * | 2021-01-18 | 2021-06-04 | 福建阿石创新材料股份有限公司 | Rotary silicon target material capable of being uniformly sputtered and preparation method thereof |
| 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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