CN106191792A - Work method prepared by a kind of modified tungsten niobium alloy target - Google Patents
Work method prepared by a kind of modified tungsten niobium alloy target Download PDFInfo
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- CN106191792A CN106191792A CN201610656572.4A CN201610656572A CN106191792A CN 106191792 A CN106191792 A CN 106191792A CN 201610656572 A CN201610656572 A CN 201610656572A CN 106191792 A CN106191792 A CN 106191792A
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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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of modified tungsten niobium alloy target and prepare work method, processing technology is simple, quality of finished product good, high comprehensive performance, makes target material surface metalized modified with physical gas-phase deposite method, solves tungsten niobium alloy target surface metalation this difficult problem modified.
Description
Technical field
The present invention relates to alloy material and manufacture field, be specifically related to a kind of modified tungsten niobium alloy 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 target, described target is generally made up of sputtering target material and penstock, compared with flat target, the utilization rate of target higher and
After sputtering, quality of forming film is more preferable, has huge development potentiality in target market.Tungsten niobium hard alloy has high intensity, height firmly
The features such as degree, excellent wearability, thermostability and good corrosion resistance, are therefore widely used in high pressure, high rotating speed, height
The working environments such as temperature, Korrosionsmedium.
For now, tungsten niobium target is not only to compactness, hardness with the highest requirement can be had, simultaneously to material by processing type
Interior tissue uniformity also have 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
There is technology the part non-sputtered region of target can be carried out blasting treatment, the so part surface through sandblasting and become coarse, enter
And become easily to adsorb deposit, reduce peeling phenomenon odds.
Summary of the invention
The present invention provides a kind of modified tungsten niobium alloy target to prepare work method, and processing technology is simple, and quality of finished product good is comprehensive
Can be excellent, make target material surface metalized modified with physical gas-phase deposite method, solve tungsten niobium alloy target surface metalation modified
This difficult problem.
To achieve these goals, the invention provides a kind of modified tungsten niobium alloy target and prepare work method, the method includes
Following steps:
(1) target is prepared
Using tungsten powder and niobium powder for making raw material, its each constituent mass percentage ratio is tungsten powder: 85%-95%, niobium powder: 5%-15%；
Described tungsten powder purity >=99.99%, granularity are 2-3 μm, and described niobium powder purity >=99.99%, granularity are 3-8 μm；
The raw material choosing aforementioned proportion loads batch mixer, and batch mixer adjustment of rotational speed to 1000-1500 turns/min, and start rotates forward
After 6-8h, invert 10-15h, shut down afterwards powder is standby；
Being loaded in tubular rubber die sleeve by gained powder, be pressed with cold isostatic press, pressure is 250-300MPa, pressure
Target material blank body is obtained standby after 20-40 minute processed；
Gained target material blank body is put in sintering furnace heat up stage by stage, heat preservation sintering, the first stage: risen to 700 by room temperature
DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C；Second stage: risen to 1000 DEG C by 700 DEG C, the heating-up time is
4h, furnace temperature is incubated 2h after rising to 1000 DEG C；Phase III: risen to 1250 DEG C by 1000 DEG C, the heating-up time is 2h, and furnace temperature rises to
1h it is incubated after 1250 DEG C；Fourth stage: risen to 1600 DEG C by 1250 DEG C, the heating-up time is 5h, and furnace temperature is incubated after rising to 1600 DEG C
2h；In 5th stage: risen to 1850 DEG C by 1600 DEG C, the heating-up time is 2h, and furnace temperature is incubated 4h after rising to 2000 DEG C；The most sintered
After journey completes, take out gained metal body, use recirculated water cooling down to standby after room temperature；
Metal body after being cooled down by gained is heated to 1350 DEG C-1600 DEG C, and is maintained in this temperature range to enter it
Row hot rolling processes, and after its thickness is rolled to 5-100mm, naturally cools to room temperature, obtains target blank；
The surfaces externally and internally of gained target blank is carried out rough turn, fine grinding, obtains target；
(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 processing technology is simple, quality of finished product good, high comprehensive performance, use physical gas-phase deposite method
Make target material surface metalized modified, solve tungsten niobium alloy target surface metalation this difficult problem modified.
Detailed description of the invention
Embodiment one
Prepare target
Using tungsten powder and niobium powder for making raw material, its each constituent mass percentage ratio is tungsten powder 95%, niobium powder: 5%；Described tungsten powder is pure
Degree >=99.99%, granularity are 2-3 μm, and described niobium powder purity >=99.99%, granularity are 3-8 μm；Choose the raw material of aforementioned proportion
Load batch mixer, by batch mixer adjustment of rotational speed to 1000 turn/min, after start rotates forward 6h, invert 10h, shut down afterwards powder is standby
With.
Being loaded in tubular rubber die sleeve by gained powder, be pressed with cold isostatic press, pressure is 250MPa, pressure
Target material blank body is obtained standby after making 20 minutes.
Gained target material blank body is put in sintering furnace heat up stage by stage, heat preservation sintering, the first stage: risen to by room temperature
700 DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C；Second stage: risen to 1000 DEG C by 700 DEG C, the heating-up time
For 4h, furnace temperature is incubated 2h after rising to 1000 DEG C；Phase III: risen to 1250 DEG C by 1000 DEG C, the heating-up time is 2h, and furnace temperature rises to
1h it is incubated after 1250 DEG C；Fourth stage: risen to 1600 DEG C by 1250 DEG C, the heating-up time is 5h, and furnace temperature is incubated after rising to 1600 DEG C
2h；In 5th stage: risen to 1850 DEG C by 1600 DEG C, the heating-up time is 2h, and furnace temperature is incubated 4h after rising to 2000 DEG C；The most sintered
After journey completes, take out gained metal body, use recirculated water cooling down to standby after room temperature.
Metal body after being cooled down by gained is heated to 1350 DEG C, and is maintained in this temperature range it is carried out heat
Roll process, after its thickness is rolled to 5-100mm, naturally cool to room temperature, obtain target blank；Interior appearance by gained target blank
Face carries out rough turn, fine grinding, obtains target.
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
Using tungsten powder and niobium powder for making raw material, its each constituent mass percentage ratio is tungsten powder: 85%, niobium powder: 15%；Described tungsten
Powder purity >=99.99%, granularity are 2-3 μm, and described niobium powder purity >=99.99%, granularity are 3-8 μm；Choose the former of aforementioned proportion
Material loads batch mixer, by batch mixer adjustment of rotational speed to 1500 turn/min, after start rotates forward 8h, inverts 15h, shuts down to obtain powder afterwards
Expect standby.
Being loaded in tubular rubber die sleeve by gained powder, be pressed with cold isostatic press, pressure is 300MPa, pressure
Target material blank body is obtained standby after making 40 minutes.
Gained target material blank body is put in sintering furnace heat up stage by stage, heat preservation sintering, the first stage: risen to by room temperature
700 DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C；Second stage: risen to 1000 DEG C by 700 DEG C, the heating-up time
For 4h, furnace temperature is incubated 2h after rising to 1000 DEG C；Phase III: risen to 1250 DEG C by 1000 DEG C, the heating-up time is 2h, and furnace temperature rises to
1h it is incubated after 1250 DEG C；Fourth stage: risen to 1600 DEG C by 1250 DEG C, the heating-up time is 5h, and furnace temperature is incubated after rising to 1600 DEG C
2h；In 5th stage: risen to 1850 DEG C by 1600 DEG C, the heating-up time is 2h, and furnace temperature is incubated 4h after rising to 2000 DEG C；The most sintered
After journey completes, take out gained metal body, use recirculated water cooling down to standby after room temperature.
Metal body after being cooled down by gained is heated to 1350 DEG C-1600 DEG C, and right in being maintained at this temperature range
It carries out hot rolling process, after its thickness is rolled to 5-100mm, naturally cools to room temperature, obtains target blank；By gained target blank
Surfaces externally and internally carry out rough turn, fine grinding, obtain target.
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. a work method prepared by modified tungsten niobium alloy target, and the method comprises the steps:
(1) target is prepared
Using tungsten powder and niobium powder for making raw material, its each constituent mass percentage ratio is tungsten powder: 85%-95%, niobium powder: 5%-15%；
Described tungsten powder purity >=99.99%, granularity are 2-3 μm, and described niobium powder purity >=99.99%, granularity are 3-8 μm；
The raw material choosing aforementioned proportion loads batch mixer, and batch mixer adjustment of rotational speed to 1000-1500 turns/min, and start rotates forward
After 6-8h, invert 10-15h, shut down afterwards powder is standby；
Being loaded in tubular rubber die sleeve by gained powder, be pressed with cold isostatic press, pressure is 250-300MPa, pressure
Target material blank body is obtained standby after 20-40 minute processed；
Gained target material blank body is put in sintering furnace heat up stage by stage, heat preservation sintering, the first stage: risen to 700 by room temperature
DEG C, the heating-up time is 5h, and furnace temperature is incubated 7h after rising to 700 DEG C；Second stage: risen to 1000 DEG C by 700 DEG C, the heating-up time is
4h, furnace temperature is incubated 2h after rising to 1000 DEG C；Phase III: risen to 1250 DEG C by 1000 DEG C, the heating-up time is 2h, and furnace temperature rises to
1h it is incubated after 1250 DEG C；Fourth stage: risen to 1600 DEG C by 1250 DEG C, the heating-up time is 5h, and furnace temperature is incubated after rising to 1600 DEG C
2h；In 5th stage: risen to 1850 DEG C by 1600 DEG C, the heating-up time is 2h, and furnace temperature is incubated 4h after rising to 2000 DEG C；The most sintered
After journey completes, take out gained metal body, use recirculated water cooling down to standby after room temperature；
Metal body after being cooled down by gained is heated to 1350 DEG C-1600 DEG C, and is maintained in this temperature range to enter it
Row hot rolling processes, and after its thickness is rolled to 5-100mm, naturally cools to room temperature, obtains target blank；
The surfaces externally and internally of gained target blank is carried out rough turn, fine grinding, obtains target；
(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)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610656572.4A CN106191792A (en) | 2016-08-12 | 2016-08-12 | Work method prepared by a kind of modified tungsten niobium alloy target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610656572.4A CN106191792A (en) | 2016-08-12 | 2016-08-12 | Work method prepared by a kind of modified tungsten niobium alloy target |
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| CN106191792A true CN106191792A (en) | 2016-12-07 |
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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 |
| 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 |
-
2016
- 2016-08-12 CN CN201610656572.4A patent/CN106191792A/en active Pending
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 |
| 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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Application publication date: 20161207 |