CN106119788A - 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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- CN106119788A CN106119788A CN201610656528.3A CN201610656528A CN106119788A CN 106119788 A CN106119788 A CN 106119788A CN 201610656528 A CN201610656528 A CN 201610656528A CN 106119788 A CN106119788 A CN 106119788A
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- tungsten
- nickel
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- target
- heat treatment
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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
Abstract
The invention discloses a kind of modified tungsten nickel target and prepare work method, first use isostatic cool pressing technique that tungsten, nickel mixed-powder and rustless steel hollow pipe are carried out densification first and preforming, form half fine and close tungsten, nickel mixed-powder and rustless steel initial blank, make follow-up heat and other static pressuring processes that tungsten, nickel mixed-powder and rustless steel initial blank can be carried out more preferable densification, make target material surface metalized modified with physical gas-phase deposite method, solve tungsten nickel this difficult problem of target material surface metalized modified.
Description
Technical field
The present invention relates to alloy material and manufacture field, be specifically related to a kind of modified tungsten nickel target and prepare work method.
Background technology
In recent years, growing along with sputtering target material and sputtering technology, sputtering target material serves more in sputtering technology
Carrying out the most important effect, 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, described pipe target is generally made up of sputtering target material and penstock, compared with flat target, the utilization rate of pipe target higher and
After sputtering, quality of forming film is more preferable, has huge development potentiality in target market.
W-Ni hard alloy has high intensity, high rigidity, excellent wearability, thermostability and good corrosion resistance etc.
Feature, is therefore widely used in the working environments such as high pressure, high rotating speed, high temperature, Korrosionsmedium.Owing to Ni belongs to face-centered cubic
(F.c.c) crystallographic system, plasticity is fine, is susceptible to plastic deformation during wet grinding, forms the Ni powder ball of lamellar.
Tungsten nickel target is a kind of more typical alloy target material of ratio, and tungsten nickel has low-resistance coefficient, and good is thermally-stabilised
Property and non-oxidizability；Meanwhile, good processability, the feature that toughness is high, therefore former using tungsten, nickel mixed-powder as sputtering target material
Material, one of tungsten nickel pipe target pipe target having become semiconductor applications large usage quantity being made up of both raw materials.For now, use
In the tungsten nickel pipe target of semiconductor manufacturing not only to compactness, hardness with the highest requirement can be had, simultaneously to material by processing type
Interior tissue uniformity also has the highest requirement.
Owing to, in sputter procedure, the edge of target can leave the particulate matter that sputtering produces, these particulate matters are gradually
Accumulation becomes deposit.Deposit gathers on target and peeling phenomenon (peeling) can occur the most afterwards, sinking of peeling
Long-pending thing not only can affect sputtering environment, is also easy to drop on product surface, causes that product is defective even to be scrapped.To this end, it is existing
Having technology can be modified the part non-sputtered region of target processing, so part surface through sandblasting becomes coarse, enters
And become easily to adsorb deposit, reduce peeling phenomenon odds.
Summary of the invention
The present invention provides a kind of modified tungsten nickel target to prepare work method, first uses isostatic cool pressing technique to mix tungsten, nickel
Close powder and rustless steel hollow pipe carries out densification first and preforming, form half fine and close tungsten, nickel mixed-powder and rustless steel
Initial blank, makes follow-up heat and other static pressuring processes can preferably cause tungsten, nickel mixed-powder and rustless steel initial blank
Close, make target material surface metalized modified with physical gas-phase deposite method, solve tungsten nickel target material surface metalized modified this
A difficult problem.
To achieve these goals, the invention provides a kind of modified tungsten nickel target and prepare work method, the method bag
Include following steps:
(1) target is prepared
Thering is provided tungsten and nickel mixed-powder, the mass ratio of described tungsten powder and nikel powder is 9.95:1 to 10.05:1；
Described tungsten and nickel mixed-powder are carried out isostatic cool pressing technique, forms tungsten and nickel mixed-powder initial blank；
Described tungsten and nickel mixed-powder initial blank are loaded vacuum canning and to described vacuum canning evacuation after, to described tungsten
Carry out heat and other static pressuring processes with nickel mixing initial blank, form tungsten nickel；
Remove described vacuum canning, it is thus achieved that with described tungsten nickel target；
Wherein, the technological temperature of described isostatic cool pressing technique is 50 DEG C to 150 DEG C, and environmental stress is 170MPa to 190MPa,
Process time under described technological temperature and environmental stress is 15 minutes to 25 minutes；
Wherein, described heat and other static pressuring processes includes heating technique and HIP sintering technique；
The technological temperature of described heating technique is 300 DEG C to 400 DEG C, at said temperatures insulation 5 hours to 7 hours；
The technological temperature of described HIP sintering technique is 1150 DEG C to 1250 DEG C, and environmental stress is 160MPa to 200MPa,
Process time under described technological temperature and environmental stress is 5 hours to 7 hours；
(2) modification
Coating chamber at Pvd equipment loads metal or alloy cathode targets, is then put into by cubic boron nitride micropowder
Drum-type deposition table；Close coating chamber door, set vapour deposition parameter, carry out physical vapor deposition coating film；
Cubic boron nitride micropowder after plated film is carried out heat treatment in vacuum heat treatment furnace, i.e. obtains surface metalation modification
Tungsten nickel target.
Preferably, in described step (2), Fisher particle size≤3.0 μm of the cubic boron nitride micropowder of employing；
The parameter of processes of physical vapor deposition is set as: take out base vacuum in advance to 3.0 × 10-3Below Pa, is passed through working gas Ar
Gas, in coating process, sputtering pressure is set in 1～5Pa；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 frequency of vibration of vibrational system is 15～40Hz；Plated film
Time is 5～10h；
Described heat treatment is carried out under vacuo, and vacuum 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 temperature retention 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 use isostatic cool pressing technique to tungsten, nickel
Mixed-powder and rustless steel hollow pipe carry out densification first and preforming, form half fine and close tungsten, nickel mixed-powder and stainless
Steel initial blank, makes follow-up heat and other static pressuring processes can carry out tungsten, nickel mixed-powder and rustless steel initial blank preferably
Densification, makes target material surface metalized modified with physical gas-phase deposite method, solve tungsten nickel target material surface metalized modified this
One difficult problem.
Detailed description of the invention
Embodiment one
Prepare target
Thering is provided tungsten and nickel mixed-powder, the mass ratio of described tungsten powder and nikel powder is 9.95:1；
Described tungsten and nickel mixed-powder are carried out isostatic cool pressing technique, forms tungsten and nickel mixed-powder initial blank；
Described tungsten and nickel mixed-powder initial blank are loaded vacuum canning and to described vacuum canning evacuation after, to described tungsten
Carry out heat and other static pressuring processes with nickel mixing initial blank, form tungsten nickel；
Remove described vacuum canning, it is thus achieved that with described tungsten nickel target.
Wherein, the technological temperature of described isostatic cool pressing technique is 50 DEG C, and environmental stress is 170MPa, at described technological temperature
It it is 15 minutes with the process time under environmental stress.
Wherein, described heat and other static pressuring processes includes heating technique and HIP sintering technique；
The technological temperature of described heating technique is 300 DEG C, at said temperatures insulation 5 hours；
The technological temperature of described HIP sintering technique is 1150 DEG C, and environmental stress is 160MPa, at described technological temperature and
Process time under environmental stress is 5 hours.
Modification
Coating chamber at Pvd equipment loads metal or alloy cathode targets, is then put into by cubic boron nitride micropowder
Drum-type deposition table；Close coating chamber door, set vapour deposition parameter, carry out physical vapor deposition coating film.
Cubic boron nitride micropowder after plated film is carried out heat treatment in vacuum heat treatment furnace, i.e. obtains surface metalation and change
The tungsten nickel target of property.
Preferably, Fisher particle size≤3.0 μm of the cubic boron nitride micropowder of employing；
The parameter of processes of physical vapor deposition is set as: take out base vacuum in advance to 3.0 × 10-3Below Pa, is passed through working gas Ar
Gas, in coating process, sputtering pressure is set in 1Pa；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 frequency of vibration of vibrational system is 15Hz；The plated film time is 5h；
Described heat treatment is carried out under vacuo, and vacuum can be controlled in 1 × 10-5In the range of Pa, treatment temperature set
In the range of 500 DEG C, heat treatment temperature retention time is set as 50min, furnace cooling.
Embodiment two
Prepare target
Thering is provided tungsten and nickel mixed-powder, the mass ratio of described tungsten powder and nikel powder is 10.05:1；
Described tungsten and nickel mixed-powder are carried out isostatic cool pressing technique, forms tungsten and nickel mixed-powder initial blank；
Described tungsten and nickel mixed-powder initial blank are loaded vacuum canning and to described vacuum canning evacuation after, to described tungsten
Carry out heat and other static pressuring processes with nickel mixing initial blank, form tungsten nickel；
Remove described vacuum canning, it is thus achieved that with described tungsten nickel target.
Wherein, the technological temperature of described isostatic cool pressing technique is 150 DEG C, and environmental stress is 190MPa, at described process warm
Process time under degree and environmental stress is 25 minutes.
Wherein, described heat and other static pressuring processes includes heating technique and HIP sintering technique；
The technological temperature of described heating technique is 400 DEG C, at said temperatures insulation 7 hours；
The technological temperature of described HIP sintering technique is 1250 DEG C, and environmental stress is 200MPa, at described technological temperature and
Process time under environmental stress is 7 hours.
Modification
Coating chamber at Pvd equipment loads metal or alloy cathode targets, is then put into by cubic boron nitride micropowder
Drum-type deposition table；Close coating chamber door, set vapour deposition parameter, carry out physical vapor deposition coating film.
Cubic boron nitride micropowder after plated film is carried out heat treatment in vacuum heat treatment furnace, i.e. obtains surface metalation and change
The tungsten nickel target of property.
Preferably, Fisher particle size≤3.0 μm of the cubic boron nitride micropowder of employing；
The parameter of processes of physical vapor deposition is set as: take out base vacuum in advance to 3.0 × 10-3Below Pa, is passed through working gas Ar
Gas, in coating process, sputtering pressure is set in 5Pa；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 frequency of vibration of vibrational system is 40Hz；The plated film time is 10h；
Described heat treatment is carried out under vacuo, and vacuum can be controlled in 1 × 10-3In the range of Pa, treatment temperature set
In the range of 700 DEG C, heat treatment temperature retention time is set as 80min, furnace cooling.
Claims (2)
1. modified tungsten nickel target prepares a work method, and the method comprises the steps:
(1) target is prepared
Thering is provided tungsten and nickel mixed-powder, the mass ratio of described tungsten powder and nikel powder is 9.95:1 to 10.05:1；
Described tungsten and nickel mixed-powder are carried out isostatic cool pressing technique, forms tungsten and nickel mixed-powder initial blank；
Described tungsten and nickel mixed-powder initial blank are loaded vacuum canning and to described vacuum canning evacuation after, to described tungsten
Carry out heat and other static pressuring processes with nickel mixing initial blank, form tungsten nickel；
Remove described vacuum canning, it is thus achieved that with described tungsten nickel target；
Wherein, the technological temperature of described isostatic cool pressing technique is 50 DEG C to 150 DEG C, and environmental stress is 170MPa to 190MPa,
Process time under described technological temperature and environmental stress is 15 minutes to 25 minutes；
Wherein, described heat and other static pressuring processes includes heating technique and HIP sintering technique；
The technological temperature of described heating technique is 300 DEG C to 400 DEG C, at said temperatures insulation 5 hours to 7 hours；
The technological temperature of described HIP sintering technique is 1150 DEG C to 1250 DEG C, and environmental stress is 160MPa to 200MPa,
Process time under described technological temperature and environmental stress is 5 hours to 7 hours；
(2) modification
Coating chamber at Pvd equipment loads metal or alloy cathode targets, is then put into by cubic boron nitride micropowder
Drum-type deposition table；Close coating chamber door, set vapour deposition parameter, carry out physical vapor deposition coating film；
Cubic boron nitride micropowder after plated film is carried out heat treatment in vacuum heat treatment furnace, i.e. obtains surface metalation modification
Tungsten nickel target.
2. the method for claim 1, it is characterised in that in described step (2), the cubic boron nitride micropowder of employing
Fisher particle size≤3.0 μm；
The parameter of processes of physical vapor deposition is set as: take out base vacuum in advance to 3.0 × 10-3Below Pa, is passed through working gas Ar
Gas, in coating process, sputtering pressure is set in 1～5Pa；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 frequency of vibration of vibrational system is 15～40Hz；Plated film
Time is 5～10h；
Described heat treatment is carried out under vacuo, and vacuum 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 temperature retention time is set as 50～80min, furnace cooling.
Priority Applications (1)
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| CN201610656528.3A CN106119788A (en) | 2016-08-12 | 2016-08-12 | A kind of modified tungsten nickel target prepares work method |
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| CN201610656528.3A CN106119788A (en) | 2016-08-12 | 2016-08-12 | A kind of modified tungsten nickel target prepares work method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106735189A (en) * | 2016-11-24 | 2017-05-31 | 中国工程物理研究院材料研究所 | A kind of motlten metal cladding high temperature insostatic pressing (HIP) preparation method of particles reiforced metal-base composition |
| CN110885963A (en) * | 2019-10-09 | 2020-03-17 | 安泰天龙钨钼科技有限公司 | Tungsten-nickel alloy target material and preparation method thereof |
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| JPH03153864A (en) * | 1989-11-09 | 1991-07-01 | Nippon Shokubai Kagaku Kogyo Co Ltd | Method and device for surface coating of particle |
| US20060254903A1 (en) * | 2002-12-25 | 2006-11-16 | Takayuki Abe | Polygonal barrel spattering device, polygonal, barrel spattering method, coated particle formed by the device and method, microcapsule, and method of manufacturing the micro- capsule |
| CN102806353A (en) * | 2012-08-17 | 2012-12-05 | 苏州晶纯新材料有限公司 | Production method of molybdenum alloy tube target |
| CN106312071A (en) * | 2015-06-19 | 2017-01-11 | 宁波江丰电子材料股份有限公司 | A tungsten-titanium tube target manufacture method |
| CN106521432A (en) * | 2015-09-09 | 2017-03-22 | 北京有色金属研究总院 | Method for cubic boron nitride micro-powder particle surface metallization modifying |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03153864A (en) * | 1989-11-09 | 1991-07-01 | Nippon Shokubai Kagaku Kogyo Co Ltd | Method and device for surface coating of particle |
| US20060254903A1 (en) * | 2002-12-25 | 2006-11-16 | Takayuki Abe | Polygonal barrel spattering device, polygonal, barrel spattering method, coated particle formed by the device and method, microcapsule, and method of manufacturing the micro- capsule |
| CN102806353A (en) * | 2012-08-17 | 2012-12-05 | 苏州晶纯新材料有限公司 | Production method of molybdenum alloy tube target |
| CN106312071A (en) * | 2015-06-19 | 2017-01-11 | 宁波江丰电子材料股份有限公司 | A tungsten-titanium tube target manufacture method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106735189A (en) * | 2016-11-24 | 2017-05-31 | 中国工程物理研究院材料研究所 | A kind of motlten metal cladding high temperature insostatic pressing (HIP) preparation method of particles reiforced metal-base composition |
| CN106735189B (en) * | 2016-11-24 | 2019-01-15 | 中国工程物理研究院材料研究所 | A kind of molten metal cladding hot isostatic pressing preparation method of particles reiforced metal-base composition |
| CN110885963A (en) * | 2019-10-09 | 2020-03-17 | 安泰天龙钨钼科技有限公司 | Tungsten-nickel alloy target material and preparation method thereof |
| CN110885963B (en) * | 2019-10-09 | 2022-03-04 | 安泰天龙钨钼科技有限公司 | Tungsten-nickel alloy target material and preparation method thereof |
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