CN108239755A - A kind of modified tungsten nickel target prepares work method - Google Patents
A kind of modified tungsten nickel target prepares work method Download PDFInfo
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- CN108239755A CN108239755A CN201611212399.5A CN201611212399A CN108239755A CN 108239755 A CN108239755 A CN 108239755A CN 201611212399 A CN201611212399 A CN 201611212399A CN 108239755 A CN108239755 A CN 108239755A
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- Prior art keywords
- tungsten
- nickel
- powder
- target
- vacuum
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Classifications
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- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0647—Boron nitride
-
- 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
Abstract
The invention discloses a kind of modified tungsten nickel targets to prepare work method, first tungsten, nickel mixed-powder and stainless steel hollow pipe are carried out using isostatic cool pressing technique to be densified for the first time and preforming, form half fine and close tungsten, nickel mixed-powder and stainless steel initial blank, subsequent heat and other static pressuring processes is allow to carry out better densification to tungsten, nickel mixed-powder and stainless steel initial blank, make target material surface metalized modified, this problem of solution tungsten nickel target material surface metalized modified with physical gas-phase deposite method.
Description
Technical field
The present invention relates to alloy material manufacturing fields, and in particular to a kind of modified tungsten nickel target prepares work method.
Background technology
In recent years, growing with sputtering target material and sputtering technology, sputtering target material plays more in sputtering technology
Carry out more important role, the quality of sputtering target material has directly influenced the quality of forming film after sputtering.Sputtering target material is broadly divided into flat
Face target and pipe target, the pipe target is usually made of sputtering target material and penstock, compared with flat target, the utilization rate higher of pipe target and
Quality of forming film is more preferable after sputtering, has huge development potentiality in target market.
W-Ni hard alloy has high intensity, high rigidity, excellent wearability, heat resistance and good corrosion resistance etc.
Feature, therefore it is widely used in the working environments such as high pressure, high rotating speed, high temperature, Korrosionsmedium.Since Ni belongs to face-centered cubic
(F.c.c) crystallographic system, plasticity is fine, is easily plastically deformed during wet-milling, forms the Ni powder balls of sheet.
Tungsten nickel target is a kind of than more typical alloy target material, and tungsten nickel has low-resistance coefficient, good thermostabilization
Property and inoxidizability；Meanwhile the characteristics of processing performance is good, and toughness is high, therefore using tungsten, nickel mixed-powder as sputtering target material original
Material, tungsten nickel tube target has become one of larger pipe target of semiconductor applications dosage made of both raw materials.For now, it uses
In semiconductor manufacturing tungsten nickel tube target not only to compactness, hardness and can processing type have very high requirement, while to material
Interior tissue uniformity also has very high requirement.
Due in sputtering process, on the edge of target there are the particulate matter generated is sputtered, these particulate matters are gradual
Accumulation becomes deposit.Deposit is assembled on target can occur peeling phenomenon (peeling) afterwards to a certain extent, and peeling is sunk
Product object can not only influence to sputter environment, be also easy to fall on product surface, cause product defective or even scrap.It is for this purpose, existing
There is technology that can be modified processing to the part non-sputtered region of target, the part surface Jing Guo sandblasting in this way becomes coarse, into
And become easily to adsorb deposit, reduce peeling phenomenon odds.
Invention content
The present invention provides a kind of modified tungsten nickel target and prepares work method, and first tungsten, nickel are mixed using isostatic cool pressing technique
It closes powder and stainless steel hollow pipe carries out densification for the first time and preforming, formation half fine and close tungsten, nickel mixed-powder and stainless steel
Initial blank allows subsequent heat and other static pressuring processes preferably to cause tungsten, nickel mixed-powder and stainless steel initial blank
It is close, make target material surface metalized modified with physical gas-phase deposite method, solve tungsten nickel target material surface metalized modified this
Problem.
To achieve these goals, the present invention provides a kind of modified tungsten nickel targets to prepare work method, this method packet
Include following steps：
(1) target is prepared
The mass ratio of offer tungsten and nickel mixed-powder, the tungsten powder and nickel powder is 9.95:1 to 10.05:1；
Isostatic cool pressing technique is carried out to the tungsten and nickel mixed-powder, forms tungsten and nickel mixed-powder initial blank；
After the tungsten and nickel mixed-powder initial blank are packed into vacuum canning and the vacuum canning is vacuumized, to institute
It states tungsten and nickel mixing initial blank carries out heat and other static pressuring processes, form tungsten nickel；
The vacuum canning is removed, is obtained with the tungsten nickel target；
Wherein, the technological temperature of the isostatic cool pressing technique be 50 DEG C to 150 DEG C, environmental stress for 170MPa extremely
190MPa, the process time under the technological temperature and environmental stress are 15 minutes to 25 minutes；
Wherein, the heat and other static pressuring processes include heating process and HIP sintering technique；
The technological temperature of the heating process is 300 DEG C to 400 DEG C, keeps the temperature 5 hours to 7 hours at said temperatures；
The technological temperature of the HIP sintering technique be 1150 DEG C to 1250 DEG C, environmental stress for 160MPa extremely
200MPa, the process time under the technological temperature and environmental stress are 5 hours to 7 hours；
(2) modification
Metal or alloy cathode targets are packed into the coating chamber of Pvd equipment, then by cubic boron nitride micro mist
It is put into drum-type deposition table；Coating chamber door is closed, setting vapor deposition parameter carries out physical vapor deposition coating film；
Cubic boron nitride micro mist after plated film in vacuum heat treatment furnace is heat-treated and is changed to get to surface metalation
The tungsten nickel target of property.
Preferably, in the step (2), Fisher particle size≤3.0 μm of the cubic boron nitride micro mist of use；
The parameter setting of processes of physical vapor deposition is：Pre- base vacuum of taking out is to 3.0 × 10-3Pa is hereinafter, be passed through work gas
Body Ar gas, sputtering pressure is set in 1~5Pa in coating process；Sample heating temperature is 150~250 DEG C；Target power density model
It encloses for 10~25W/cm2；The rotating speed of drum-type deposition table is 20~35r/min；The vibration frequency of vibrational system is 15~40Hz；
Plated film time is 5~10h；
The heat treatment carries out under vacuum, and vacuum degree can be controlled in 1 × 10-5~1 × 10-3In the range of Pa, heat
Treatment temperature is set in the range of 500~700 DEG C, and heat treatment soaking time is set as 50~80min, furnace cooling.
It is an advantage of the current invention that a kind of modified tungsten nickel target prepares work method, first using isostatic cool pressing technique pair
Tungsten, nickel mixed-powder and stainless steel hollow pipe carry out densification for the first time and preforming, formed half fine and close tungsten, nickel mixed-powder and
Stainless steel initial blank allows subsequent heat and other static pressuring processes to carry out more tungsten, nickel mixed-powder and stainless steel initial blank
Good densification makes target material surface metalized modified with physical gas-phase deposite method, solves the metallization of tungsten nickel target material surface and changes
This problem of property.
Specific embodiment
Embodiment one
Prepare target
The mass ratio of offer tungsten and nickel mixed-powder, the tungsten powder and nickel powder is 9.95:1；
Isostatic cool pressing technique is carried out to the tungsten and nickel mixed-powder, forms tungsten and nickel mixed-powder initial blank；
After the tungsten and nickel mixed-powder initial blank are packed into vacuum canning and the vacuum canning is vacuumized, to institute
It states tungsten and nickel mixing initial blank carries out heat and other static pressuring processes, form tungsten nickel；
The vacuum canning is removed, is obtained with the tungsten nickel target.
Wherein, the technological temperature of the isostatic cool pressing technique is 50 DEG C, environmental stress 170MPa, in the technological temperature
It it is 15 minutes with the process time under environmental stress.
Wherein, the heat and other static pressuring processes include heating process and HIP sintering technique；
The technological temperature of the heating process is 300 DEG C, keeps the temperature 5 hours at said temperatures；
The technological temperature of the HIP sintering technique is 1150 DEG C, environmental stress 160MPa, in the process warm
Process time under degree and environmental stress is 5 hours.
Modification
Metal or alloy cathode targets are packed into the coating chamber of Pvd equipment, then by cubic boron nitride micro mist
It is put into drum-type deposition table；Coating chamber door is closed, setting vapor deposition parameter carries out physical vapor deposition coating film.
Cubic boron nitride micro mist after plated film in vacuum heat treatment furnace is heat-treated and is changed to get to surface metalation
The tungsten nickel target of property.
Preferably, Fisher particle size≤3.0 μm of the cubic boron nitride micro mist of use；
The parameter setting of processes of physical vapor deposition is：Pre- base vacuum of taking out is to 3.0 × 10-3Pa is hereinafter, be passed through work gas
Body Ar gas, sputtering pressure is set in 1Pa in coating process；Sample heating temperature is 150 DEG C；Target power density range is
10W/cm2；The rotating speed of drum-type deposition table is 20r/min；The vibration frequency of vibrational system is 15Hz；Plated film time is
5h；
The heat treatment carries out under vacuum, and vacuum degree can be controlled in 1 × 10-5In the range of Pa, heat treatment temperature
It is set in the range of 500 DEG C, heat treatment soaking time is set as 50min, furnace cooling.
Embodiment two
Prepare target
The mass ratio of offer tungsten and nickel mixed-powder, the tungsten powder and nickel powder is 10.05:1；
Isostatic cool pressing technique is carried out to the tungsten and nickel mixed-powder, forms tungsten and nickel mixed-powder initial blank；
After the tungsten and nickel mixed-powder initial blank are packed into vacuum canning and the vacuum canning is vacuumized, to institute
It states tungsten and nickel mixing initial blank carries out heat and other static pressuring processes, form tungsten nickel；
The vacuum canning is removed, is obtained with the tungsten nickel target.
Wherein, the technological temperature of the isostatic cool pressing technique is 150 DEG C, environmental stress 190MPa, in the process warm
Process time under degree and environmental stress is 25 minutes.
Wherein, the heat and other static pressuring processes include heating process and HIP sintering technique；
The technological temperature of the heating process is 400 DEG C, keeps the temperature 7 hours at said temperatures；
The technological temperature of the HIP sintering technique is 1250 DEG C, environmental stress 200MPa, in the process warm
Process time under degree and environmental stress is 7 hours.
Modification
Metal or alloy cathode targets are packed into the coating chamber of Pvd equipment, then by cubic boron nitride micro mist
It is put into drum-type deposition table；Coating chamber door is closed, setting vapor deposition parameter carries out physical vapor deposition coating film.
Cubic boron nitride micro mist after plated film in vacuum heat treatment furnace is heat-treated and is changed to get to surface metalation
The tungsten nickel target of property.
Preferably, Fisher particle size≤3.0 μm of the cubic boron nitride micro mist of use；
The parameter setting of processes of physical vapor deposition is：Pre- base vacuum of taking out is to 3.0 × 10-3Pa is hereinafter, be passed through work gas
Body Ar gas, sputtering pressure is set in 5Pa in coating process；Sample heating temperature is 250 DEG C；Target power density range is
25W/cm2；The rotating speed of drum-type deposition table is 35r/min；The vibration frequency of vibrational system is 40Hz；Plated film time is
10h；
The heat treatment carries out under vacuum, and vacuum degree can be controlled in 1 × 10-3In the range of Pa, heat treatment temperature
It is set in the range of 700 DEG C, heat treatment soaking time is set as 80min, furnace cooling.
Claims (2)
1. a kind of modified tungsten nickel target prepares work method, this method comprises the following steps：
(1) target is prepared
The mass ratio of offer tungsten and nickel mixed-powder, the tungsten powder and nickel powder is 9.95:1 to 10.05:1；
Isostatic cool pressing technique is carried out to the tungsten and nickel mixed-powder, forms tungsten and nickel mixed-powder initial blank；
After the tungsten and nickel mixed-powder initial blank are packed into vacuum canning and the vacuum canning is vacuumized, to the tungsten
Heat and other static pressuring processes are carried out with nickel mixing initial blank, form tungsten nickel；
The vacuum canning is removed, is obtained with the tungsten nickel target；
Wherein, the technological temperature of the isostatic cool pressing technique is 50 DEG C to 150 DEG C, and environmental stress is 170MPa to 190MPa,
Process time under the technological temperature and environmental stress is 15 minutes to 25 minutes；
Wherein, the heat and other static pressuring processes include heating process and HIP sintering technique；
The technological temperature of the heating process is 300 DEG C to 400 DEG C, keeps the temperature 5 hours to 7 hours at said temperatures；
The technological temperature of the HIP sintering technique is 1150 DEG C to 1250 DEG C, and environmental stress is 160MPa to 200MPa,
Process time under the technological temperature and environmental stress is 5 hours to 7 hours；
(2) modification
Metal or alloy cathode targets are packed into the coating chamber of Pvd equipment, are then put into cubic boron nitride micro mist
Drum-type deposition table；Coating chamber door is closed, setting vapor deposition parameter carries out physical vapor deposition coating film；
Cubic boron nitride micro mist after plated film is heat-treated to be modified to surface metalation in vacuum heat treatment furnace
Tungsten nickel target.
2. the method as described in claim 1, which is characterized in that in the step (2), the cubic boron nitride micro mist of use
Fisher particle size≤3.0 μm；
The parameter setting of processes of physical vapor deposition is：Pre- base vacuum of taking out is to 3.0 × 10-3Pa is hereinafter, be passed through working gas Ar
Gas, sputtering pressure is set in 1~5Pa in coating process；Sample heating temperature is 150~250 DEG C；Target power density range is
10~25W/cm2；The rotating speed of drum-type deposition table is 20~35r/min；The vibration frequency of vibrational system is 15~40Hz；Plated film
Time is 5~10h；
The heat treatment carries out under vacuum, and vacuum degree can be controlled in 1 × 10-5~1 × 10-3In the range of Pa, heat treatment
Temperature is set in the range of 500~700 DEG C, and heat treatment soaking time is set as 50~80min, furnace cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611212399.5A CN108239755A (en) | 2016-12-25 | 2016-12-25 | A kind of modified tungsten nickel target prepares work method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611212399.5A CN108239755A (en) | 2016-12-25 | 2016-12-25 | A kind of modified tungsten nickel target prepares work method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108239755A true CN108239755A (en) | 2018-07-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611212399.5A Pending CN108239755A (en) | 2016-12-25 | 2016-12-25 | A kind of modified tungsten nickel target prepares work method |
Country Status (1)
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|---|---|
| CN (1) | CN108239755A (en) |
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2016
- 2016-12-25 CN CN201611212399.5A patent/CN108239755A/en active Pending
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Application publication date: 20180703 |