CN105420678B - A kind of Al addition Ni W alloys targets and its manufacture method - Google Patents
A kind of Al addition Ni W alloys targets and its manufacture method Download PDFInfo
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Abstract
The invention discloses a kind of Al addition Ni W alloys targets and its manufacture method.The target is made up of by atomic percent following element：Al0.5 10%, W3.5 15%, Ni75~96%.Its manufacture method includes batching step successively, intermediate alloy melting step, secondary smelting, ingot casting stage, forges step, a heat treatment step, milling step, secondary heat treatment step and machining production finished product step.The Al manufactured by the inventive method, which adds Ni W alloy targets, has the advantages that finished product Composition Control is accurate, and distributed components, segregation-free, nothing are mingled with, and crystal grain is uniform, and finished product purity is high, specific as follows：Each Composition Control is accurate≤0.2at%, mean grain size is not more than 80 μm, high purity more than 99.95%.
Description
Technical field
The invention belongs to metal material and metallurgical preparation field, more particularly to a kind of Al addition Ni-W alloy target materials and its system
Method is made, it is especially suitable for magnetron sputtering.
Background technology
The world today has come into the information age.The explosive growth of information content proposes more to information storage technology
Carry out higher requirement.To high storage capacity, high data access speed, high performance price ratio storage device increasing need is entered
One step advances the development of stored record technology.In recent years, the performance more and more higher of conventional store recording technique, new storage note
Record technology continues to bring out information storage and has become one of most active field in current information technology.Stored in all information
In mode, magnetic storage technically still has suitable because it has excellent record performance, using flexible, cheap
Big development potentiality, so the major technique still stored as Contemporary Information.
The end of the year 2004, Toshiba disclose first hard disk drive based on perpendicular magnetic recording (PMR) technology of the whole world
(HDD), surface density has reached 133Gb/in2, this nearly reaches superparamagnetic limit under longitudinal magnetic recording (LMR) technical conditions.
With the development of perpendicular magnetic recording technol, surface density has reached 1Tb/in at present2, the thin film system of magnetic recording develops therewith,
The kind of required magnetic control spattering target also constantly changes.Inculating crystal layer is unusual important component in the film system of perpendicular recording,
Seed crystal is to can be used to promote the formation of monocrystal with the small crystals with required crystal phase with crystal orientation, seed crystal, and inculating crystal layer is with original
Sublayer deposition technique by seed crystal in layer be plated in substrate surface, form inculating crystal layer.At present, conventional seed crystal layer material has
NiCr systems alloy, NiW systems alloy.
For nickel-base alloy, strand is obtained frequently with vacuum melting at present, hot rolling cogging after strand is heated again, after cooling
Cold rolling simultaneously carries out recrystallization processing again.Although this method technique is simple, easily realizes, obtained material exist microsegregation,
The defects of uneven microstructure.
The report of addition Al Ni-W alloy target materials is had not yet to see, micro Al is added in Ni-W alloys to be carried
The corrosion resisting property of high Ni-W alloy firms, extend the anti-corrosion time of the alloy firm.
The content of the invention
The defects of for prior art, it is an object of the invention to provide a kind of Al addition Ni-W alloy target materials and its manufacture
Method, the finished product Composition Control for the alloy target material that this method obtains is accurate, distributed components, segregation-free, and without being mingled with, crystal grain is equal
Even, finished product purity is high, especially suitable for magnetron sputtering.
To achieve these goals, present invention employs following technical scheme：
A kind of Al adds Ni-W alloy target materials, and the alloy target material is made up of by atomic percent following element：Al0.5-
10%, W3.5-15%, Ni75~96%.Specifically, Al atomic percentage conc can be 0.9%, 1.2%, 1.5%,
2.2%th, any value in 2.9%, 3.6%, 4.5%, 5.9%, 7.1%, 8.5%, 9.5% etc.；W atomic percentage conc can
Think any in 4.0%, 5.5%, 6.9%, 7.6%, 8.5%, 9.6%, 10.5%, 11.5%, 13.1%, 14.5% etc.
Value.
In above-mentioned alloy target material, as a kind of preferred embodiment, the alloy target material is by atomic percent by following
Element forms：Al1-5%, W5-10%, Ni84-95%.
In the composition of above-mentioned alloy target material, Al can improve the corrosion resisting property of target under severe conditions, and Al content is low
When 0.5at%, the corrosion resisting property and temperature of Ni-W films improve unobvious；When Al content is higher than 10at%, Ni-W films
Corrosion resisting property can deteriorate；It is preferred that Al content is 1-5at%.
In order to manufacture above-mentioned Al additions Ni-W alloy target materials, the present invention provides a kind of manufacture method, and the manufacture method is successively
Including batching step, intermediate alloy melting step, secondary smelting, ingot casting stage, step, a heat treatment step, rolling are forged
Step, secondary heat treatment step and machining production finished product step, wherein：
In the batching step, each raw metal nickel, aluminium are weighed respectively according to the composition proportion of the alloy target material of design
And tungsten bar；
In the intermediate alloy melting step, load weighted metallic nickel and tungsten block are put into vacuum induction melting furnace
Row vacuum induction melting, wherein, smelting temperature control is at 1650~1700 DEG C, refining time 10-15min, after the completion of melting
Intermediate alloy liquid is cooled down, starts to pour when the intermediate alloy liquid temperature degree reaches 50~100 DEG C of more than the liquidus curve of Ni-W alloys
Casting, so as to obtain nickel tungsten intermediate alloy ingot blank；
In the secondary smelting, ingot casting stage, nickel tungsten intermediate alloy ingot blank is put into vacuum induction melting furnace first
Vacuum induction melting is carried out, wherein smelting temperature control is at 1650~1700 DEG C, refining time 5-10min, when refining is completed
Metal Al blocks are added in vacuum induction melting furnace by smelting furnace charging hopper, to Ni-W- after metal Al blocks all fusing
Al aluminium alloys are cooled down, when the aluminium alloy temperature in smelting furnace be cooled to more than the liquidus curve of three kinds of Ni-W-Al alloys 50~
Start to cast at 100 DEG C, obtain Ni-W-Al alloy ingot blanks；
In the forging step, Ni-W-Al alloy ingot blanks are first put into holding furnace (such as Muffle furnace, gas furnace),
2~4 hours are incubated under the conditions of 1000~1300 DEG C, then the Ni-W-Al alloy ingot blanks are forged to obtain one again
It is sized the forging stock of specification；
In a heat treatment step, the forging stock is incubated 20~36 hours under the conditions of 1100 DEG C~1350 DEG C
It is heat-treated, then air cooling, stove are cold or are quickly quenching into room temperature；
In the milling step, the forging stock after the once heat treatment is incubated 1.5 under the conditions of 1050~1300 DEG C
Hot rolling is carried out after~2.5 hours, room temperature is subsequently cooled to and carries out cold rolling at ambient temperature, the total deformation of the cold rolling is
30~50%；
In the secondary heat treatment step, the slab obtained after cold rolling is incubated 20 under the conditions of 900 DEG C~1150 DEG C
~120 minutes, air cooling of coming out of the stove；
In the machining production finished product step, by the Ni-W-Al alloys slab after secondary heat treatment by size requirement
It is machined to finished product.
In the above-mentioned methods, using vacuum induction melting, the introducing of field trash can be avoided；After forging, forging stock is carried out
High temperature solution treated is the once heat treatment of the present invention, can eliminate component segregation；Cold rolling is carried out after hot rolling, ensures that cold rolling has and is more than
30% deflection is with Broken Crystal；Recrystallization processing secondary heat treatment i.e. of the invention is carried out after cold rolling should to remove alloy
Power, control heterogeneous microstructure, control crystallite dimension.The Al obtained by the above method adds the purity ＞ of Ni-W alloy target materials
99.95%, mean grain size is controlled within 80 μm, no component segregation.
The above method is illustrated in order to more detailed, the above method can be illustratively described as：
In the intermediate alloy melting step, the smelting temperature may be controlled to 1650 DEG C, 1660 DEG C, 1670 DEG C,
1680 DEG C or 1690 DEG C, the smelting time is that refining time can be 10min, 12min, 13min, 14min or 15min,
Intermediate alloy fluid temperature after melting is carried out when reaching more than Ni-W aluminium alloy phase lines 55 DEG C, 65 DEG C, 70 DEG C, 80 DEG C or 95 DEG C
Casting；
In the secondary smelting, ingot casting stage, the smelting temperature may be controlled to 1650 DEG C, 1660 DEG C, 1670 DEG C,
1680 DEG C or 1690 DEG C, the smelting time can be 5min, 7min, 8min, 9min, the alloy liquid temperature when in smelting furnace
Degree is cast when being cooled to more than the liquidus curve of three kinds of Ni-W-Al alloys 55 DEG C, 65 DEG C, 70 DEG C, 80 DEG C or 95 DEG C；
In the forging step, Ni-W-Al alloy ingot blanks are first put into holding furnace (such as Muffle furnace, gas furnace),
2~4 hours are incubated under the conditions of 1000~1300 DEG C, then the Ni-W-Al alloy ingot blanks are forged to obtain one again
It is sized the forging stock of specification；
In the forging step, the Ni-W-Al alloy ingot blanks can be at 1050 DEG C, 1100 DEG C, 1150 DEG C, 1200 DEG C
Or 2h, 2.5h, 3h or 4h are incubated under the conditions of 1250 DEG C；As the dimensions of above-mentioned forging stock, it is directed to depending on the demand of client
, such as can be 218*174*35.5mm slab；
In a heat treatment step, the forging stock at 1150 DEG C, 1200 DEG C, 1220 DEG C, 1260 DEG C, 1290 DEG C or
20h, 23h, 28h, 32h, 35h or 36h hour are incubated under the conditions of 1315 DEG C；
In the milling step, by once be heat-treated after forging stock 1070 DEG C, 1090 DEG C, 1120 DEG C, 1122 DEG C,
Hot rolling is carried out after being incubated 1.5h, 2.0h or 2.5h under the conditions of 1170 DEG C, 1190 DEG C, 1230 DEG C or 1270 DEG C, is subsequently cooled to room
Temperature simultaneously carries out cold rolling at ambient temperature, and the total deformation of the cold rolling can be 32%, 37%, 42%, 45%, 48%；
In the secondary heat treatment step, the slab that is obtained after the cold rolling 900 DEG C, 1000 DEG C, 1030 DEG C, 1060
DEG C, 1090 DEG C, be incubated 30min, 60min, 70min, 90min or 110min under the conditions of 1120 DEG C or 1150 DEG C.
In the above-mentioned methods, as a kind of preferred embodiment, in the intermediate alloy melting step and described secondary molten
In refining, ingot casting stage, the vacuum of the vacuum induction melting is below 0.1Pa.
In the above-mentioned methods, as a kind of preferred embodiment, in the forging step, the Ni-W-Al alloy pigs
Base is incubated under the conditions of 1070-1270 DEG C.
In the above-mentioned methods, as a kind of preferred embodiment, in a heat treatment step, the forging stock is existed
It is incubated under the conditions of 1220 DEG C~1320 DEG C.
In the above-mentioned methods,, will be after the once heat treatment in the milling step as a kind of preferred embodiment
Forging stock be put into be incubated in the Muffle furnace of steel rolling heating under the conditions of 1070-1270 DEG C after carry out hot rolling；It is highly preferred that by described in
Forging stock after being once heat-treated is put into the Muffle furnace of steel rolling heating to be carried out after insulation 1.8-2.2h under the conditions of 1100-1200 DEG C
Hot rolling.
In the above-mentioned methods, as a kind of preferred embodiment, in the milling step, the passage of the hot rolling is 2-
3 passages, hot rolling total deformation are controlled in 50-65%, and the deformation amount controlling of each passage of hot rolling is between 20%~25%；It is described cold
The total deformation rolled is 40~45%, and each pass deformation of the cold rolling is controlled between 8-10%.
In the above-mentioned methods, as a kind of preferred embodiment, in the secondary heat treatment step, will be obtained after cold rolling
Slab be incubated 60~120 minutes under the conditions of 1000 DEG C~1150 DEG C.
In the above-mentioned methods, as a kind of preferred embodiment, in the batching step, the purity of the raw metal
More than 99.95%.
For prior art, the present invention has following beneficial effect：The present invention has finished product Composition Control essence
Really, the advantages that distributed components, segregation-free, nothing are mingled with, and crystal grain is uniform, and finished product purity is high.Above-mentioned advantage is specific as follows：Alloy
In each Composition Control it is accurate≤0.2at%, mean grain size is not more than 80 μm, high purity more than 99.95%, non-in target
The content of metal impurities oxygen is less than 50ppm, the content of carbon is less than 20ppm.The target is especially suitable for magnetron sputtering.
Brief description of the drawings
Fig. 1 is the metallographic structure figure for the Al addition Ni-W alloy target materials that the embodiment of the present invention 1 obtains.
Fig. 2 is the ESEM back scattering figure for the Al addition Ni-W alloy target materials that the embodiment of the present invention 1 obtains.
Fig. 3 is the ESEM back scattering figure for the Al addition Ni-W alloy target materials that the embodiment of the present invention 5 obtains.
Fig. 4 is the metallographic structure figure for the Al addition Ni-W alloy target materials that the embodiment of the present invention 6 obtains.
Fig. 5 is the ESEM back scattering figure for the Al addition Ni-W alloy target materials that comparative example 1 obtains.
Fig. 6 is the ESEM back scattering figure for the Al addition Ni-W alloy target materials that comparative example 2 obtains.
Embodiment
With reference to specific embodiment, the present invention is described in detail, but the present invention is not limited thereto.
Following six embodiment is that the manufacture method that Ni-W alloy target materials are added according to Al of the present invention is prepared respectively
The 6 batches of Ni-W-Al alloy disks.
Embodiment 1
Ni-W-Al alloy disks manufactured in the present embodiment are made up of by atomic percent following element：Ni：89.5%, W：
10%, Al：0.5%.
The specification of alloy disks manufactured in the present embodiment is 170 × 6.35mm of Φ.
Manufacture method is as follows：
(1) dispensing：The nickel block of purity 99.95%, purity 99.95% are weighed by the design requirement of above-mentioned alloy target material composition
High-purity aluminium block and purity 99.95% high-purity tungsten bar；
(2) intermediate alloy melting：The nickel weighed up and tungsten metal derby are put into vacuum induction melting furnace, smelted by normal
Vacuum degree control is in below 0.1Pa, melting temperature when technique smelting (being smelted by technique well known in the art), wherein melting
Degree control has a power failure at 1690 DEG C or so, refining time 15min, after the completion of melting cools down intermediate alloy liquid, when middle aluminium alloy
Temperature starts to cast when reaching 1600 DEG C, so as to obtain nickel tungsten intermediate alloy ingot blank；
(3) secondary smelting, casting：Intermediate alloy ingot blank is put into vacuum induction melting furnace, while metal Al blocks are put into
In smelting furnace charging hopper, smelted by normal smelting process in (being smelted by technique well known in the art) smelting furnace
Vacuum degree control is in below 0.1Pa during intermediate alloy ingot, wherein melting, and smelting temperature control is at 1690 DEG C or so, refining time
For 10min, metal Al blocks are added before the cooling that has a power failure when refining is completed, have a power failure cooling after metal Al blocks all fusing, until nickel
Partinium liquid temperature degree starts to cast when reaching 1590 DEG C, obtains nickel partinium ingot blank；
(4) forge：Nickel partinium ingot blank obtained by melting is put into Muffle furnace, carried out after being incubated 4 hours at 1200 DEG C
Hot forging, obtain the slab of 218*174*35.5mm specifications；
(5) once it is heat-treated：Slab after forging is put into Muffle furnace, is incubated 30 hours at 1300 DEG C, then stove is cold
To room temperature；
(6) roll：Slab after being once heat-treated is put into the Muffle furnace of steel rolling heating, it is small in 1240 DEG C of insulations 1.5
When after carry out 3 passages of hot rolling, (pass deformation of the present embodiment is 20% left to pass deformation between 20%~25%
It is right), obtain the slab of 455*176*15.5mm specifications；Then room temperature and cold rolling at room temperature are naturally cooled to, passage during cold rolling
Deflection is 8%~10%, and total deformation 40%, the specification of slab is 995*177*8.5mm after cold rolling；
(7) secondary heat treatment：The slab rolled is put into Muffle furnace, is incubated 70 minutes at 1100 DEG C, air cooling of coming out of the stove；
(8) machine：By the Ni-W-Al alloys slab after secondary heat treatment by size requirement machine, first wire cutting into
The disk of given size, then with Vehicle Processing into the Ni-W-Al alloy target materials for meeting dimensional accuracy.
Alloy target material end properties manufactured in the present embodiment is referring to table 1, and its metallographic structure figure is referring to Fig. 1.
It can be seen from figure 1 that crystal grain is uniform, mean grain size is less than 80 μm；It can be seen in fig. 2 that target finished product is inclined without composition
Analysis.
Embodiment 2
Ni-W-Al alloy disks manufactured in the present embodiment are made up of by atomic percent following element：Ni：82%, W：
8%, Al：10%.
The specification of alloy disks manufactured in the present embodiment is 170 × 6.35mm of Φ.
Manufacture method is as follows：
(1) dispensing：The nickel block of purity 99.95%, purity 99.95% are weighed by the design requirement of above-mentioned alloy target material composition
High-purity aluminium block and purity 99.95% high-purity tungsten bar；
(2) intermediate alloy melting：The nickel weighed up and tungsten metal derby are put into vacuum induction melting furnace, smelted by normal
Vacuum degree control is in 0.085Pa, smelting temperature when technique smelting (being smelted by technique well known in the art), wherein melting
Control has a power failure at 1650 DEG C or so, refining time 15min, after the completion of melting cools down intermediate alloy liquid, when middle aluminium alloy temperature
Degree starts to cast when reaching 1600 DEG C, so as to obtain nickel tungsten intermediate alloy ingot blank；
(3) secondary smelting, casting：Intermediate alloy ingot blank is put into vacuum induction melting furnace, while metal Al blocks are put into
In smelting furnace charging hopper, smelted by normal smelting process in (being smelted by technique well known in the art) smelting furnace
Vacuum degree control is in 1650 DEG C or so, refining time in 0.085Pa, smelting temperature control during intermediate alloy ingot, wherein melting
10min, metal Al blocks are added before the cooling that has a power failure when refining is completed, the cooling that has a power failure after metal Al blocks all fusing is until nickel tungsten aluminium
Aluminium alloy temperature starts to cast when reaching 1540 DEG C, obtains nickel partinium ingot blank；
(4) forge：Ingot blank obtained by melting is put into Muffle furnace, hot forging is carried out after being incubated 4 hours at 1070 DEG C, obtains
218*174*35.5mm the slab of specification；
(5) once it is heat-treated：Slab after forging is put into Muffle furnace, is incubated 20 hours at 1320 DEG C, then air cooling
To room temperature；
(6) roll：Slab after being once heat-treated is put into the Muffle furnace of steel rolling heating, 2 hours are incubated at 1070 DEG C
After carry out 3 passage hot rollings, pass deformation (pass deformation of the present embodiment is 20% or so) between 20%~25%, obtain
To the slab of 455*176*15.5mm specifications；Then room temperature and cold rolling at room temperature are naturally cooled to, pass deformation during cold rolling
For 8%~10%, total deformation 40%, the specification of slab is 995*177*8.5mm after cold rolling；
(7) secondary heat treatment：The slab rolled is put into Muffle furnace, is incubated 60 minutes at 1150 DEG C, air cooling of coming out of the stove；
(8) machine：By the Ni-W-Al alloys slab after secondary heat treatment by size requirement machine, first wire cutting into
The disk of given size, then with Vehicle Processing into the Ni-W-Al alloy target materials for meeting dimensional accuracy.
Alloy target material end properties manufactured in the present embodiment is uniform referring to table 1, the alloy grain；In addition, the embodiment
The ESEM back scattering figure of obtained alloy target material is identical with the ESEM back scattering figure of the alloy target material of embodiment 1, target
Finished product is still without component segregation, because the ESEM back scattering figure that two embodiments obtain is essentially identical, so the present embodiment
ESEM back scattering figure does not repeat to provide.
Embodiment 3
Ni-W-Al alloy disks manufactured in the present embodiment are made up of by atomic percent following element：Ni：93.5%, W：
3.5%, Al：3%.
The specification of alloy disks manufactured in the present embodiment is 170 × 6.35mm of Φ.
Manufacture method is as follows：(1) dispensing：The nickel of purity 99.95% is weighed by the design requirement of above-mentioned alloy target material composition
High-purity tungsten bar of block, high-purity aluminium block of purity 99.95% and purity 99.95%；
(2) intermediate alloy melting：The nickel weighed up and tungsten metal derby are put into vacuum induction melting furnace, smelted by normal
Vacuum degree control is in 0.08Pa, smelting temperature when technique smelting (being smelted by technique well known in the art), wherein melting
Control has a power failure at 1680 DEG C or so, refining time 10min, after the completion of melting cools down intermediate alloy liquid, when middle aluminium alloy temperature
Degree starts to cast when reaching 1595 DEG C, so as to obtain nickel tungsten intermediate alloy ingot blank；
(3) secondary smelting, casting：Intermediate alloy ingot blank is put into vacuum induction melting furnace, while metal Al blocks are put into
In smelting furnace charging hopper, smelted by normal smelting process in (being smelted by technique well known in the art) smelting furnace
Vacuum degree control is in 1680 DEG C or so, refining time in 0.08Pa, smelting temperature control during intermediate alloy ingot, wherein melting
8min, metal Al blocks are added before the cooling that has a power failure when refining is completed, the cooling that has a power failure after metal Al blocks all fusing is until nickel tungsten aluminium
Aluminium alloy temperature starts to cast when reaching 1580 DEG C, obtains nickel partinium ingot blank；
(4) forge：Ingot blank obtained by melting is put into Muffle furnace, hot forging is carried out after being incubated 2 hours at 1270 DEG C, obtains
218*174*35.5mm the slab of specification；
(5) once it is heat-treated：Slab after forging is put into Muffle furnace, is incubated 35 hours at 1270 DEG C, then stove is cold
To room temperature；
(6) roll：Slab after being once heat-treated is put into the Muffle furnace of steel rolling heating, it is small in 1270 DEG C of insulations 1.5
When after carry out 2 passage hot rollings, pass deformation (pass deformation of the present embodiment is 25% or so) between 20%~25%,
Obtain the slab of 455*176*15.5mm specifications；Then room temperature and cold rolling at room temperature are naturally cooled to, passage deforms during cold rolling
Measure as 8%~10%, total deformation 50%, the specification of slab is 1080*177*7.8mm after cold rolling；
(7) secondary heat treatment：The slab rolled is put into Muffle furnace, is incubated 120 minutes at 1000 DEG C, sky of coming out of the stove
It is cold；
(8) machine：By the Ni-W-Al alloys slab after secondary heat treatment by size requirement machine, first wire cutting into
The disk of given size, then with Vehicle Processing into the Ni-W-Al alloy target materials for meeting dimensional accuracy.
Alloy target material end properties manufactured in the present embodiment is referring to table 1, and the alloy grain is uniform, in addition, the embodiment
The ESEM back scattering figure of the ESEM back scattering figure of obtained alloy target material and the alloy target material of embodiment 1 also basic phase
Together, target finished product does not also repeat to provide still without component segregation in the ESEM back scattering figure of this present embodiment.
Embodiment 4
Ni-W-Al alloy disks manufactured in the present embodiment are made up of by atomic percent following element：Ni：80%, W：
15%, Al：5%.
The specification of alloy disks manufactured in the present embodiment is 170 × 6.35mm of Φ.
Manufacture method is as follows：
(1) dispensing：The nickel block of purity 99.95%, purity 99.95% are weighed by the design requirement of above-mentioned alloy target material composition
High-purity aluminium block and purity 99.95% high-purity tungsten bar；
(2) intermediate alloy melting：The nickel weighed up and tungsten metal derby are put into vacuum induction melting furnace, smelted by normal
Vacuum degree control is in 0.05Pa, smelting temperature when technique smelting (being smelted by technique well known in the art), wherein melting
Control has a power failure at 1680 DEG C or so, refining time 12min, after the completion of melting cools down intermediate alloy liquid, when middle aluminium alloy temperature
Degree starts to cast when reaching 1600 DEG C, so as to obtain nickel tungsten intermediate alloy ingot blank；
(3) secondary smelting, casting：Intermediate alloy ingot blank is put into vacuum induction melting furnace, while metal Al blocks are put into
In smelting furnace charging hopper, smelted by normal smelting process in (being smelted by technique well known in the art) smelting furnace
Vacuum degree control is in 1680 DEG C or so, refining time in 0.05Pa, smelting temperature control during intermediate alloy ingot, wherein melting
8min, metal Al blocks are added before the cooling that has a power failure when refining is completed, the cooling that has a power failure after metal Al blocks all fusing is until nickel tungsten aluminium
Aluminium alloy temperature starts to cast when reaching 1580 DEG C, obtains nickel partinium ingot blank；
(4) forge：Ingot blank obtained by melting is put into Muffle furnace, hot forging is carried out after being incubated 3 hours at 1200 DEG C, obtains
218*174*35.5mm the slab of specification；
(5) once it is heat-treated：Slab after forging is put into Muffle furnace, is incubated 36 hours at 1220 DEG C, then air cooling
To room temperature；
(6) roll：Slab after being once heat-treated is put into the Muffle furnace of steel rolling heating, it is small in 1270 DEG C of insulations 1.5
When after carry out hot rolling, pass deformation (pass deformation of the present embodiment is 25% or so) between 20%~25%, obtain
455*176*15.5mm the slab of specification；Then room temperature and cold rolling at room temperature are naturally cooled to, pass deformation is during cold rolling
8%~10%, total deformation 50%, the specification of slab is 1080*177*7.8mm after cold rolling；
(7) secondary heat treatment：The slab rolled is put into Muffle furnace, is incubated 70 minutes at 1000 DEG C, air cooling of coming out of the stove；
(8) machine：By the Ni-W-Al alloys slab after secondary heat treatment by size requirement machine, first wire cutting into
The disk of given size, then with Vehicle Processing into the Ni-W-Al alloy target materials for meeting dimensional accuracy.
Alloy target material end properties manufactured in the present embodiment is referring to table 1, and the alloy grain is uniform, in addition, the embodiment
The ESEM back scattering figure of the ESEM back scattering figure of obtained alloy target material and the alloy target material of embodiment 1 also basic phase
Together, target finished product does not also repeat to provide still without component segregation in the ESEM back scattering figure of this present embodiment.
Embodiment 5
The alloy target material composition and size of preparation are same as Example 1.
Preparation method, in addition to the temperature that step (5) is once heat-treated is changed into 1100 DEG C from 1300 DEG C, other operating procedures
With embodiment 1.
The alloy target material end properties that the embodiment obtains is referring to table 1.Its ESEM back scattering figure referring to Fig. 3, from
Understood in Fig. 3, the composition for the target finished product that the present embodiment obtains slightly is segregated, but not serious.
Embodiment 6
The alloy target material composition and size of preparation are same as Example 1.
Preparation method, except in step (6) control of cold rolling total deformation for 30% and meanwhile appropriate adjustment hot rolling deformation amount with
Outside, other operating procedures are the same as embodiment 1.
The alloy target material end properties that the embodiment obtains is referring to table 1.Obtained grain structure is uneven, and crystal grain chi
It is very little larger to see Fig. 4.
Comparative example 1
The alloy target material composition and size of preparation are same as Example 1.
Preparation method：In addition to step (2) and (3), other operating procedures are same as Example 1；
In this comparative example, the step (2) in embodiment 1 and (3) are revised as：Raw metal nickel, aluminium and tungsten bar is complete
Portion is put into vacuum induction melting furnace, smelts (being smelted by technique well known in the art) melting by normal smelting process
Vacuum degree control is in 1690 DEG C or so, refining time in 0.1Pa, smelting temperature control during raw metal, wherein melting in stove
10min, power failure cooled alloy liquid starts to cast when nickel partinium liquid temperature degree reaches 1580 DEG C after refining, obtains nickel tungsten aluminium
Alloy ingot blank；The alloy target material end properties that this comparative example obtains is referring to table 1.As can be seen from Fig. 5, the presence of target finished product is tighter
The component segregation of weight, wherein, white point W segregations, and Al scaling loss is more.
Comparative example 2
The alloy target material composition and size of preparation are same as Example 1.
Preparation method：In addition to a heat treatment step is not carried out, other operating procedures are same as Example 1.
The alloy target material end properties that this comparative example obtains is referring to table 1.As can be seen from Fig. 6, the presence of target finished product is tighter
The component segregation of weight.
All of above embodiment product is on magnetron sputtering apparatus, under identical process conditions, is sunk on Si substrates
Film has been accumulated, and corrosion resistance test has been carried out with reference to the neutral salt spray test method (NSS) in national standard GB/T2423.17-2008,
Testing time is 16h, 24h, 48h, 96h, 168h, 336h, 672h, to there is corrosion failure as anti-corrosion time, anti-corrosion time
Such as table 1.
The properties of product table of the embodiment of the present invention of table 1
The method of testing of properties of product is as follows described in table 1：
Composition tolerances be by the different parts of same finished product target sample carry out alloy component analysis after obtain,
Alloy component analysis use energy dispersion X-ray spectrometer (EDX) or Xray fluorescence spectrometer (XRF).
The measure of purity is determined using ICP or GDMS methods.
Mean grain size is calculated by GB/T6394-2002 (mean grain size is graded (resection)).
The test of corrosion resisting property is with reference to GB/T2423.17-2008, electric and electronic product environmental test, part 2:Experiment
Method test Ka：Salt fog.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to the protection model of the limitation present invention
Enclose.In addition, it should also be understood that, after the technology contents of the present invention have been read, those skilled in the art can make each to the present invention
Kind change, modification and/or variation, all these equivalent form of values equally fall within the guarantor that the application appended claims are limited
Within the scope of shield.
Claims (10)
- A kind of 1. manufacture method of Al additions Ni-W alloy target materials, it is characterised in thatThe Al additions Ni-W alloy target materials are made up of by atomic percent following element：Al 0.5-10%, W 3.5-15%, Ni 75~96%；The manufacture method of the Al additions Ni-W alloy target materials, it is secondary molten including batching step, intermediate alloy melting step successively Refining, ingot casting stage, forge step, a heat treatment step, milling step, secondary heat treatment step and machining production finished product step Suddenly, wherein：In the batching step, according to the composition proportion of the alloy target material of design weigh respectively each raw metal nickel, aluminium and Tungsten bar；In the intermediate alloy melting step, load weighted metallic nickel and tungsten block are put into vacuum induction melting furnace and carried out very Empty induction melting, wherein, smelting temperature is controlled at 1650~1700 DEG C, refining time 10-15min, is cooled down after the completion of melting Intermediate alloy liquid, start to cast when the intermediate alloy liquid temperature degree reaches 50~100 DEG C of more than the liquidus curve of Ni-W alloys, from And obtain nickel tungsten intermediate alloy ingot blank；In the secondary smelting, ingot casting stage, nickel tungsten intermediate alloy ingot blank is put into vacuum induction melting furnace carried out first Vacuum induction melting, wherein smelting temperature are controlled at 1650~1700 DEG C, refining time 5-10min, and refining passes through when completing Smelting furnace charging hopper adds metal Al blocks in vacuum induction melting furnace, and Ni-W-Al is closed after metal Al blocks all fusing Golden liquid is cooled down, when the aluminium alloy temperature in smelting furnace is cooled to 50~100 DEG C of more than the liquidus curve of three kinds of Ni-W-Al alloys When start to cast, obtain Ni-W-Al alloy ingot blanks；In the forging step, Ni-W-Al alloy ingot blanks are first put into holding furnace, are incubated under the conditions of 1000~1300 DEG C 2~4 hours, then the Ni-W-Al alloy ingot blanks are forged to obtain the forging stock of certain size specification again；In a heat treatment step, the forging stock is incubated 20~36 hours under the conditions of 1100 DEG C~1350 DEG C and carried out Heat treatment, then air cooling, stove are cold or are quickly quenching into room temperature；In the milling step, the forging stock after the once heat treatment is incubated 1.5~2.5 under the conditions of 1050~1300 DEG C Carry out hot rolling after hour, be subsequently cooled to room temperature and carry out cold rolling at ambient temperature, the total deformation of the cold rolling for 30~ 50%；In the secondary heat treatment step, the slab obtained after cold rolling is incubated 20~120 under the conditions of 900 DEG C~1150 DEG C Minute, air cooling of coming out of the stove；In the machining production finished product step, the Ni-W-Al alloys slab after secondary heat treatment is added by size requirement machine Work is into finished product.
- 2. the manufacture method of Al additions Ni-W alloy target materials according to claim 1, it is characterised in thatThe Al additions Ni-W alloy target materials are made up of by atomic percent following element：Al 1-5%, W 5-10%, Ni 84 ~95%.
- 3. the manufacture method of Al additions Ni-W alloy target materials according to claim 1 or 2, it is characterised in thatIn the intermediate alloy melting step and the secondary smelting, ingot casting stage, the vacuum of the vacuum induction melting For below 0.1Pa.
- 4. the manufacture method of Al additions Ni-W alloy target materials according to claim 1 or 2, it is characterised in that in the forging Make in step, the Ni-W-Al alloy ingot blanks are incubated under the conditions of 1070-1270 DEG C.
- 5. the manufacture method of Al additions Ni-W alloy target materials according to claim 1 or 2, it is characterised in that described one In secondary heat treatment step, the forging stock is incubated under the conditions of 1220 DEG C~1320 DEG C.
- 6. the manufacture method of Al additions Ni-W alloy target materials according to claim 1 or 2, it is characterised in that rolled described In step processed, the forging stock after the once heat treatment is put into the Muffle furnace of steel rolling heating and protected under the conditions of 1070-1270 DEG C Hot rolling is carried out after temperature.
- 7. the manufacture method of Al additions Ni-W alloy target materials according to claim 6, it is characterised in that once hot by described in Forging stock after processing is put into the Muffle furnace of steel rolling heating carries out hot rolling after insulation 1.8-2.2h under the conditions of 1100-1200 DEG C.
- 8. the manufacture method of Al additions Ni-W alloy target materials according to claim 1 or 2, it is characterised in that rolled described In step processed, the passage of the hot rolling is 2-3 passages, and hot rolling total deformation is controlled in 50-65%, the deflection of each passage of hot rolling Control is between 20%~25%；The total deformation of the cold rolling is 40~45%, and each pass deformation of the cold rolling controls Between 8-10%.
- 9. manufacture method according to claim 1 or 2, it is characterised in that in the secondary heat treatment step, by cold rolling The slab obtained afterwards is incubated 60~120 minutes under the conditions of 1000 DEG C~1150 DEG C.
- 10. manufacture method according to claim 1 or 2, it is characterised in that in the batching step, the metal raw The purity of material is more than 99.95%.
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| TWI684658B (en) * | 2016-12-06 | 2020-02-11 | 光洋應用材料科技股份有限公司 | Co-cr-pt-based alloy sputtering target and method of preparing the same |
| CN109881048B (en) * | 2019-02-28 | 2021-09-21 | 北京理工大学 | Preparation method of high-strength high-plasticity Ni-W-X alloy |
| CN110227906A (en) * | 2019-05-08 | 2019-09-13 | 东莞市欧莱溅射靶材有限公司 | A kind of corronil rotary target material and its production method |
| CN116732479A (en) * | 2023-07-28 | 2023-09-12 | 宁波江丰电子材料股份有限公司 | Manufacturing method of integrated high-purity aluminum target for LCD |
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| JP2009155722A (en) * | 2007-12-05 | 2009-07-16 | Hitachi Metals Ltd | Ni-W BASED SINTERED TARGET MATERIAL |
| CN103221999A (en) * | 2010-11-22 | 2013-07-24 | 山阳特殊制钢株式会社 | Alloy for seed layer of magnetic recording medium, and sputtering target material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2009155722A (en) * | 2007-12-05 | 2009-07-16 | Hitachi Metals Ltd | Ni-W BASED SINTERED TARGET MATERIAL |
| CN103221999A (en) * | 2010-11-22 | 2013-07-24 | 山阳特殊制钢株式会社 | Alloy for seed layer of magnetic recording medium, and sputtering target material |
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