CN106756826A - A kind of high-purity tantalum ruthenium alloy target and preparation method thereof - Google Patents
A kind of high-purity tantalum ruthenium alloy target and preparation method thereof Download PDFInfo
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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
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- 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
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- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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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
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Abstract
The present invention provides a kind of high-purity tantalum ruthenium alloy target and preparation method thereof, ruthenium powder and tantalum powder by ruthenium powder that commercially available purity is 99.9% and tantalum powder respectively through vacuum high-temperature sublimation purification to purity more than 99.995%, through ball milling mixing after, be pressed into bulk through isostatic cool pressing, vacuum-sintering melting, high-purity tantalum ruthenium alloy ingot is obtained, then high-purity tantalum ruthenium alloy ingot is through horizontal hot forging, annealing, hot rolling, cold rolling, recrystallization annealing temperature treatment obtains high-purity tantalum ruthenium alloy target.The purifying technique of ruthenium powder of the invention and tantalum powder is simple, and purification purity is high, depth removal Ca, Cr, Co, Cu, Cd, Cl, Fe, K, Li, Mg, Na, Ni, and the target material composition of preparation is uniform, purity is high, crystal grain is tiny, and oxygen content is low, and area is big, thickness of thin.
Description
Technical field
The invention belongs to noble metal powder metallurgical technology field, and in particular to a kind of high-purity tantalum ruthenium alloy target and its system
Preparation Method.
Background technology
In recent years, with the fast development of electronics and information industry, integrated circuit sputtering target material has also obtained larger hair
Exhibition.For in the metal targets for manufacturing semiconductor chip, the sputtering target material founded the factory to have the non-ferrous metals such as thallium, titanium, aluminium, chromium and copper,
But with the height scale development of integrated arc, the metal such as aluminium, copper easily interconnects electromigration causes ic failure, because
This, requirement higher is proposed to aspects such as the purity for sputtering target material, size and heterogeneous microstructures.
Ruthenium is the very special element of property in platinum group metal, with fusing point it is high, hardness is big, be difficult the spies such as machining
Point, tantalum has high conductivity, high thermal stability and excellent decay resistance, so pure ruthenium target and pure tantalum target are integrated
It has been widely applied in circuit.But, with the increase of target size, the reduction of line width, electric conductivity based on conductor and
From the aspect of the matching performance of barrier layer, the target of ruthenium tantalum alloy has more obvious compared to pure ruthenium target and pure tantalum target
Advantage, but technology in terms of the target based on ruthenium tantalum alloy and be not as so ripe as pure ruthenium target and pure tantalum target.
A kind of tantalum ruthenium alloy target and preparation method thereof, purity is more than disclosed in Chinese patent CN 104233205B
After ruthenium powder mixing of 99.95% tantalum powder and purity more than 99.95%, bulk is pressed into through isostatic cool pressing, vacuum-sintering melting is obtained
To high-purity tantalum ruthenium alloy ingot, then, through radial direction hot forging, annealing is radially upset, annealing for high-purity tantalum ruthenium alloy ingot,
Hot rolling, cold rolling, recrystallization annealing temperature treatment, obtains high-purity tantalum ruthenium alloy target, but what the high-purity tantalum ruthenium alloy target was selected
The purity of ruthenium powder and tantalum powder is not high, although the purifying technique carried out during preparation, but will certainly influence the thin of alloy
Degree and the uniformity.Applicant of the present invention is improved on this basis, first with metal Ru and tantalum and impurity element boiling point-
Steam difference and concentration gradient, make volatile impurity element partial sublimation or evaporation, depth removal Ca, Cr, Co, Cu, Cd,
Cl, Fe, K, Li, Mg, Na, Ni, so as to be met the high purity metal ruthenium and metal tantalum powder of sputtering target material, then incite somebody to action both
Warm forging is carried out, the more preferable high-purity purity tantalum ruthenium alloy target of performance is prepared.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of high-purity tantalum ruthenium alloy target and preparation method thereof, will be commercially available
Purity be 99.9% ruthenium powder and tantalum powder respectively through vacuum high-temperature sublimation purification to purity more than 99.995% ruthenium powder and tantalum
Powder, through ball milling mixing after, be pressed into bulk through isostatic cool pressing, vacuum-sintering melting obtains high-purity tantalum ruthenium alloy ingot, then high-purity
Degree tantalum ruthenium alloy ingot is through horizontal hot forging, and annealing, hot rolling is cold rolling, and recrystallization annealing temperature treatment obtains high-purity tantalum ruthenium alloy target
Material.The purifying technique of ruthenium powder of the invention and tantalum powder is simple, and purification purity is high, depth removal Ca, Cr, Co, Cu, Cd, Cl, Fe,
K, Li, Mg, Na, Ni, the target material composition of preparation is uniform, purity is high, crystal grain is tiny, and oxygen content is low, and area is big, thickness of thin.
In order to solve the above technical problems, the technical scheme is that：
A kind of high-purity tantalum ruthenium alloy target, it is characterised in that the raw material of the high-purity tantalum ruthenium alloy target is purity
The ta powder of metal Ru powder and purity more than 99.995% more than 99.995%, metal of the purity more than 99.995%
Ruthenium powder is obtained through vacuum high-temperature sublimation purification, and ta powder of the purity more than 99.995% is obtained through vacuum high-temperature sublimation purification
Arrive, the vacuum of the vacuum high-temperature distillation is 10-2~10-4Pa, temperature is 1100-1600 DEG C, and the time is 12-24h.
As the preferred of above-mentioned technical proposal, the raw material of the purification be the metal Ru powder that commercially available purity is 99.9% and
Commercially available purity is 99.9% ta powder.
The present invention also provides a kind of preparation method of high-purity tantalum ruthenium alloy target, comprises the following steps：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, high temperature distillation under vacuum, taking-up is obtained
Metal Ru powder of the purity more than 99.995%；
(2) in ta powder that purity is 99.9% being added into tantalum container, high temperature distillation under vacuum, taking-up is obtained
Ta powder of the purity more than 99.995%；
(3) ta powder that metal Ru powder prepared by step (1) is prepared with step (2) is mixed, in vacuum ball grinder
After well mixed, carry out isostatic cool pressing and be pressed into bulk, vacuum-sintering melting obtains high-purity tantalum ruthenium alloy ingot；
(4), through horizontal hot forging, annealing, hot rolling is cold rolling, crystallization for the high-purity tantalum ruthenium alloy ingot for preparing step (3)
Annealing, obtains high-purity tantalum ruthenium alloy target.
Used as the preferred of above-mentioned technical proposal, in the step (1), elemental gas C content is not more than in metal Ru powder
60ppm, O content is not more than 50ppm.
Used as the preferred of above-mentioned technical proposal, in the step (2), elemental gas C content is not more than in ta powder
60ppm, O content is not more than 50ppm.
Used as the preferred of above-mentioned technical proposal, in the step (1) or step (2), the vacuum of vacuum condition is 10-2
~10-4Pa, the temperature of high temperature distillation is 1100-1600 DEG C, and the time of high temperature distillation is 12-24h.
As the preferred of above-mentioned technical proposal, in the step (3), the atomicity percentage of metal Ru powder and ta powder
It is 30-65at%：35-70at%.
Used as the preferred of above-mentioned technical proposal, in the step (3), vacuum is 0.3-4Pa, temperature in vacuum-sintering melting
It is 3000 DEG C to spend, and the time is 3-4h.
Used as the preferred of above-mentioned technical proposal, in the step (4), the temperature of hot rolling is 800-1000 DEG C, cold rolling temperature
It is 10-30 DEG C to spend, and the temperature of recrystallization annealing temperature treatment is 800-900 DEG C.
Used as the preferred of above-mentioned technical proposal, in the step (4), high-purity tantalum ruthenium alloy target is round pie, high-purity
The diameter for spending tantalum ruthenium alloy target is not less than 100mm, and thickness is 9-10mm.
Compared with prior art, the invention has the advantages that：
(1) present invention prepare high-purity tantalum ruthenium alloy target raw material for purity more than 99.995% metal Ru powder and
Ta powder of the purity more than 99.995%, the metal of metal Ru powder of the purity more than 99.995% and purity more than 99.995%
Tantalum powder is purified using vacuum high-temperature sublimation method, using metal Ru and the boiling point-steam difference and concentration of tantalum and impurity element
Gradient, makes volatile impurity element partial sublimation or evaporation, depth removal Ca, Cr, Co, Cu, Cd, Cl, Fe, K, Li, Mg,
Na, Ni, so as to be met the metal Ru and metal tantalum powder of sputtering target material, high-purity tantalum ruthenium alloy target are prepared after being
Lay good basis.
(2) present invention prepare high-purity tantalum ruthenium alloy target raw material for purity more than 99.995% metal Ru powder and
Ta powder of the purity more than 99.995% is purified using vacuum high-temperature sublimation method, and preferably vacuum is 10-2~10-4Pa, temperature
It is 1100-1600 DEG C to spend, and the time is 12-24h, and research finds that temperature is less than 1100 DEG C, and refining effect is not obvious, and temperature exceedes
1600 DEG C, the powder after heat treatment occurs hardened, and new pollution can be brought after crushing again, and the time is less than 12h, refining effect
Fall flat, temperature is higher than 24h, impurity element rate of sublimation regional stability reduces purification efficiency, can increase and be purified to
This.
(3) high-purity tantalum ruthenium alloy target prepared by the present invention uses ball mill by the metal Ru powder and metal tantalum of high-purity
Powder is well mixed, then metal Ru powder and ta powder generation tantalum ruthenium alloy ingot are further improved into purity, reduces oxygen content, then lead to
Horizontal hot forging is crossed, annealing, hot rolling is cold rolling, recrystallization annealing temperature treatment makes the crystal grain in high-purity tantalum ruthenium alloy target smaller,
Density is higher, and the area of the high-purity tantalum ruthenium alloy target of present invention preparation is big, thickness of thin.
Specific embodiment
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples of the invention and explanation
It is for explaining the present invention but not as a limitation of the invention.
Embodiment 1：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, 10-2It is high with 1100 DEG C under Pa vacuum conditions
Temperature rise China 12h, taking-up obtains the metal Ru powder that particle diameter of the purity more than 99.995% is 2 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(2) in ta powder that purity is 99.9% being added into tantalum container, 10-2It is high with 1100 DEG C under Pa vacuum conditions
Temperature rise China 12h, taking-up obtains the ta powder that particle diameter of the purity more than 99.995% is 2 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(3) it is 30at% according to the atomicity percentage of metal Ru powder and ta powder：70at%, by metal Ru powder and
Ta powder mixes, and with rotating speed as 200rpm, 2h is mixed in vacuum ball grinder to uniform, carries out isostatic cool pressing and is pressed into bulk,
The vacuum-sintering melting 3h at 0.3Pa and 3000 DEG C, obtains high-purity tantalum ruthenium alloy ingot.
(4) high-purity tantalum ruthenium alloy ingot is first preheated to 900 DEG C, laterally impact hot forging is carried out to high-purity tantalum ruthenium alloy,
It is the height reduction of tantalum ruthenium alloy ingot, cross-sectional area increase is to slowly warm up to 1000 DEG C, is incubated 2h, is naturally cooling to room temperature and enters
Row annealing, hot rolling is carried out being warming up to 800 DEG C, then cold rolling, then the recrystallization annealing temperature treatment 1h at 800 DEG C at 10 DEG C, from
Room temperature so is cooled to, high-purity tantalum ruthenium alloy target is obtained, high-purity tantalum ruthenium alloy target is round pie, high-purity tantalum ruthenium alloy
The diameter of target is not less than 100mm, and thickness is 9mm.
Embodiment 2：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, 10-3It is high with 1300 DEG C under Pa vacuum conditions
Temperature rise China 16h, taking-up obtains the metal Ru powder that particle diameter of the purity more than 99.995% is 1 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(2) in ta powder that purity is 99.9% being added into tantalum container, 10-3It is high with 1300 DEG C under Pa vacuum conditions
Temperature rise China 16h, taking-up obtains the ta powder that particle diameter of the purity more than 99.995% is 1 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(3) it is 65at% according to the atomicity percentage of metal Ru powder and ta powder：35at%, by metal Ru powder and
Ta powder mixes, and with rotating speed as 500rpm, 3h is mixed in vacuum ball grinder to uniform, carries out isostatic cool pressing and is pressed into bulk,
The vacuum-sintering melting 4h at 4Pa and 3000 DEG C, obtains high-purity tantalum ruthenium alloy ingot.
(4) high-purity tantalum ruthenium alloy ingot is first preheated to 900 DEG C, laterally impact hot forging is carried out to high-purity tantalum ruthenium alloy,
It is the height reduction of tantalum ruthenium alloy ingot, cross-sectional area increase is to slowly warm up to 1300 DEG C, is incubated 2h, is naturally cooling to room temperature and enters
Row annealing, hot rolling is carried out being warming up to 1000 DEG C, then cold rolling, then the recrystallization annealing temperature treatment 1h at 900 DEG C at 30 DEG C, from
Room temperature so is cooled to, high-purity tantalum ruthenium alloy target is obtained, high-purity tantalum ruthenium alloy target is round pie, high-purity tantalum ruthenium alloy
The diameter of target is not less than 100mm, and thickness is 10mm.
Embodiment 3：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, 10-4It is high with 1600 DEG C under Pa vacuum conditions
Temperature rise China 24h, taking-up obtains the metal Ru powder that particle diameter of the purity more than 99.995% is 0.5 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(2) in ta powder that purity is 99.9% being added into tantalum container, 10-4It is high with 1600 DEG C under Pa vacuum conditions
Temperature rise China 24h, taking-up obtains the ta powder that particle diameter of the purity more than 99.995% is 0.5 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(3) it is 40at% according to the atomicity percentage of metal Ru powder and ta powder：60at%, by metal Ru powder and
Ta powder mixes, and with rotating speed as 300rpm, 2.5h is mixed in vacuum ball grinder to uniform, carries out isostatic cool pressing and is pressed into block
Shape, the vacuum-sintering melting 3.5h at 0.8Pa and 3000 DEG C obtains high-purity tantalum ruthenium alloy ingot.
(4) high-purity tantalum ruthenium alloy ingot is first preheated to 900 DEG C, laterally impact hot forging is carried out to high-purity tantalum ruthenium alloy,
It is the height reduction of tantalum ruthenium alloy ingot, cross-sectional area increase is to slowly warm up to 1200 DEG C, is incubated 2h, is naturally cooling to room temperature and enters
Row annealing, hot rolling is carried out being warming up to 900 DEG C, then cold rolling, then the recrystallization annealing temperature treatment 1h at 850 DEG C at 20 DEG C, from
Room temperature so is cooled to, high-purity tantalum ruthenium alloy target is obtained, high-purity tantalum ruthenium alloy target is round pie, high-purity tantalum ruthenium alloy
The diameter of target is not less than 100mm, and thickness is 9.5mm.
Embodiment 4：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, 2 × 10-3Under Pa vacuum conditions, with 1500 DEG C
High temperature distillation 14h, taking-up obtains the metal Ru powder that particle diameter of the purity more than 99.995% is 0.8 μm, and elemental gas C content is little
In 60ppm, O content is not more than 50ppm.
(2) in ta powder that purity is 99.9% being added into tantalum container, 5 × 10-3Under Pa vacuum conditions, with 1200 DEG C
High temperature distillation 18h, taking-up obtains the ta powder that particle diameter of the purity more than 99.995% is 1.2 μm, and elemental gas C content is little
In 60ppm, O content is not more than 50ppm.
(3) it is 35at% according to the atomicity percentage of metal Ru powder and ta powder：65at%, by metal Ru powder and
Ta powder mixes, and with rotating speed as 450rpm, 2h is mixed in vacuum ball grinder to uniform, carries out isostatic cool pressing and is pressed into bulk,
The vacuum-sintering melting 3h at 1.2Pa and 3000 DEG C, obtains high-purity tantalum ruthenium alloy ingot.
(4) high-purity tantalum ruthenium alloy ingot is first preheated to 900 DEG C, laterally impact hot forging is carried out to high-purity tantalum ruthenium alloy,
It is the height reduction of tantalum ruthenium alloy ingot, cross-sectional area increase is to slowly warm up to 1100 DEG C, is incubated 2h, is naturally cooling to room temperature and enters
Row annealing, hot rolling is carried out being warming up to 950 DEG C, then cold rolling, then the recrystallization annealing temperature treatment 1h at 800 DEG C at 25 DEG C, from
Room temperature so is cooled to, high-purity tantalum ruthenium alloy target is obtained, high-purity tantalum ruthenium alloy target is round pie, high-purity tantalum ruthenium alloy
The diameter of target is not less than 100mm, and thickness is 9.2mm.
Embodiment 5：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, 10-4It is high with 1300 DEG C under Pa vacuum conditions
Temperature rise China 20h, taking-up obtains the metal Ru powder that particle diameter of the purity more than 99.995% is 0.6 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(2) in ta powder that purity is 99.9% being added into tantalum container, 5 × 10-3Under Pa vacuum conditions, with 1500 DEG C
High temperature distillation 20h, taking-up obtains the ta powder that particle diameter of the purity more than 99.995% is 0.9 μm, and elemental gas C content is little
In 60ppm, O content is not more than 50ppm.
(3) it is 45at% according to the atomicity percentage of metal Ru powder and ta powder：55at%, by metal Ru powder and
Ta powder mixes, and with rotating speed as 400rpm, 3h is mixed in vacuum ball grinder to uniform, carries out isostatic cool pressing and is pressed into bulk,
The vacuum-sintering melting 4h at 1.5Pa and 3000 DEG C, obtains high-purity tantalum ruthenium alloy ingot.
(4) high-purity tantalum ruthenium alloy ingot is first preheated to 900 DEG C, laterally impact hot forging is carried out to high-purity tantalum ruthenium alloy,
It is the height reduction of tantalum ruthenium alloy ingot, cross-sectional area increase is to slowly warm up to 1100 DEG C, is incubated 2h, is naturally cooling to room temperature and enters
Row annealing, hot rolling is carried out being warming up to 950 DEG C, then cold rolling, then the recrystallization annealing temperature treatment 1h at 800 DEG C at 15 DEG C, from
Room temperature so is cooled to, high-purity tantalum ruthenium alloy target is obtained, high-purity tantalum ruthenium alloy target is round pie, high-purity tantalum ruthenium alloy
The diameter of target is not less than 100mm, and thickness is 9.7mm.
Embodiment 6：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, 10-2It is high with 1600 DEG C under Pa vacuum conditions
Temperature rise China 24h, taking-up obtains the metal Ru powder of particle diameter 0.7 μm of the purity more than 99.995%, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(2) in ta powder that purity is 99.9% being added into tantalum container, 10-4It is high with 1100 DEG C under Pa vacuum conditions
Temperature rise China 12h, taking-up obtains the ta powder that particle diameter of the purity more than 99.995% is 1.5 μm, and elemental gas C content is not more than
60ppm, O content is not more than 50ppm.
(3) it is 65at% according to the atomicity percentage of metal Ru powder and ta powder：35at%, by metal Ru powder and
Ta powder mixes, and with rotating speed as 200rpm, 3h is mixed in vacuum ball grinder to uniform, carries out isostatic cool pressing and is pressed into bulk,
The vacuum-sintering melting 4h at 0.3Pa and 3000 DEG C, obtains high-purity tantalum ruthenium alloy ingot.
(4) high-purity tantalum ruthenium alloy ingot is first preheated to 900 DEG C, laterally impact hot forging is carried out to high-purity tantalum ruthenium alloy,
It is the height reduction of tantalum ruthenium alloy ingot, cross-sectional area increase is to slowly warm up to 1300 DEG C, is incubated 2h, is naturally cooling to room temperature and enters
Row annealing, hot rolling is carried out being warming up to 800 DEG C, then cold rolling, then the recrystallization annealing temperature treatment 1h at 800 DEG C at 30 DEG C, from
Room temperature so is cooled to, high-purity tantalum ruthenium alloy target is obtained, high-purity tantalum ruthenium alloy target is round pie, high-purity tantalum ruthenium alloy
The diameter of target is not less than 100mm, and thickness is 9.2mm.
After testing, the result of the content of each impurity element is as follows in the high-purity tantalum ruthenium alloy target that prepared by embodiment 1-6
It is shown：
As seen from the above table, the content of high-purity tantalum ruthenium alloy target impurity prepared by the present invention is all very small, tantalum ruthenium alloy
Purity it is high, and after tested find tantalum ruthenium alloy in crystallite dimension be less than 100 μm.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (10)
1. a kind of high-purity tantalum ruthenium alloy target, it is characterised in that：The raw material of the high-purity tantalum ruthenium alloy target is that purity is big
In 99.995% ta powder of metal Ru powder and purity more than 99.995%, metal Ru of the purity more than 99.995%
Powder is obtained through vacuum high-temperature sublimation purification, and ta powder of the purity more than 99.995% is obtained through vacuum high-temperature sublimation purification
Arrive, the vacuum of the vacuum high-temperature distillation is 10-2~10-4Pa, temperature is 1100-1600 DEG C, and the time is 12-24h.
2. a kind of high-purity tantalum ruthenium alloy target according to claim 1, it is characterised in that：The raw material of the purification is city
The purity sold is 99.9% metal Ru powder and ta powder that commercially available purity is 99.9%.
3. a kind of preparation method of high-purity tantalum ruthenium alloy target, it is characterised in that comprise the following steps：
(1) in metal Ru powder that purity is 99.9% being added into tantalum container, high temperature distillation under vacuum, taking-up obtains purity
Metal Ru powder more than 99.995%；
(2) in ta powder that purity is 99.9% being added into tantalum container, high temperature distillation under vacuum, taking-up obtains purity
Ta powder more than 99.995%；
(3) ta powder that metal Ru powder prepared by step (1) is prepared with step (2) is mixed, is mixed in vacuum ball grinder
After uniform, carry out isostatic cool pressing and be pressed into bulk, vacuum-sintering melting obtains high-purity tantalum ruthenium alloy ingot；
(4), through horizontal hot forging, annealing is laterally upset, annealing for the high-purity tantalum ruthenium alloy ingot for preparing step (3),
Hot rolling, cold rolling, recrystallization annealing temperature treatment, obtains high-purity tantalum ruthenium alloy target.
4. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
(1) in, elemental gas C content is not more than 60ppm in metal Ru powder, and O content is not more than 50ppm.
5. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
(2) in, elemental gas C content is not more than 60ppm in ta powder, and O content is not more than 50ppm.
6. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
(1) or in step (2), the vacuum of vacuum condition is 10-2~10-4Pa, the temperature of high temperature distillation is 1100-1600 DEG C, high
The time of temperature rise China is 12-24h.
7. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
(3) in, metal Ru powder is 30-65at% with the atomicity percentage of ta powder：35-70at%.
8. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
(3) in, vacuum is 0.3-4Pa in vacuum-sintering melting, and temperature is 3000 DEG C, and the time is 3-4h.
9. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
(4) in, the temperature of hot rolling is 800-1000 DEG C, and cold rolling temperature is 10-30 DEG C, and the temperature of recrystallization annealing temperature treatment is 800-900
℃。
10. a kind of high-purity tantalum ruthenium alloy target preparation method according to claim 3, it is characterised in that：The step
Suddenly in (4), high-purity tantalum ruthenium alloy target is round pie, and the diameter of high-purity tantalum ruthenium alloy target is not less than 100mm, and thickness is
9-10mm。
Priority Applications (1)
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| CN108754436A (en) * | 2018-06-25 | 2018-11-06 | 河南科技大学 | A kind of vacuum heating-press sintering preparation method of High-purity Tantalum ruthenium alloy target |
| CN112111714A (en) * | 2020-09-16 | 2020-12-22 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-aluminum alloy sputtering target material |
| WO2022004354A1 (en) * | 2020-06-30 | 2022-01-06 | 株式会社フルヤ金属 | Sputtering target and method for manufacturing same |
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Cited By (4)
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| CN108754436A (en) * | 2018-06-25 | 2018-11-06 | 河南科技大学 | A kind of vacuum heating-press sintering preparation method of High-purity Tantalum ruthenium alloy target |
| WO2022004354A1 (en) * | 2020-06-30 | 2022-01-06 | 株式会社フルヤ金属 | Sputtering target and method for manufacturing same |
| CN112111714A (en) * | 2020-09-16 | 2020-12-22 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-aluminum alloy sputtering target material |
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