US20070098590A1 - Ni-pt alloy and target comprising the alloy - Google Patents

Ni-pt alloy and target comprising the alloy Download PDF

Info

Publication number
US20070098590A1
US20070098590A1 US10/596,671 US59667105A US2007098590A1 US 20070098590 A1 US20070098590 A1 US 20070098590A1 US 59667105 A US59667105 A US 59667105A US 2007098590 A1 US2007098590 A1 US 2007098590A1
Authority
US
United States
Prior art keywords
alloy
high purity
purity
target
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US10/596,671
Inventor
Yuichiro Shindo
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JX Nippon Mining and Metals Corp
Nippon Mining Holdings Inc
Original Assignee
Nikko Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nikko Materials Co Ltd filed Critical Nikko Materials Co Ltd
Assigned to NIKKO MATERIALS CO., LTD. reassignment NIKKO MATERIALS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SHINDO, YUICHIRO
Assigned to NIPPON MINING & METALS CO., LTD. reassignment NIPPON MINING & METALS CO., LTD. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: NIKKO MATERIALS CO., LTD.
Publication of US20070098590A1 publication Critical patent/US20070098590A1/en
Assigned to NIPPON MINING HOLDINGS, INC. reassignment NIPPON MINING HOLDINGS, INC. MERGER (SEE DOCUMENT FOR DETAILS). Assignors: NIPPON MINING & METALS CO., LTD.
Assigned to JX NIPPON MINING & METALS CORPORATION reassignment JX NIPPON MINING & METALS CORPORATION CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: NIPPON MINING HOLDINGS, INC.
Priority to US12/957,013 priority Critical patent/US7959782B2/en
Abandoned legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • 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
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/28008—Making conductor-insulator-semiconductor electrodes
    • H01L21/28017—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon
    • H01L21/28026—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon characterised by the conductor
    • H01L21/28088—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon characterised by the conductor the final conductor layer next to the insulator being a composite, e.g. TiN

Definitions

  • the present invention relates to a Ni—Pt alloy superior in workability, a sputtering target manufacturing by rolling a Ni—Pt alloy ingot, and a manufacturing method of such Ni—Pt alloy and Ni—Pt alloy target.
  • Ni—Pt is used as a sputtering target for semiconductor devices, and this Ni—Pt target was conventionally manufactured with the powder metallurgy process. In other words, the target was manufactured by sintering Ni powder and Pt powder, or by sintering Ni—Pt alloy powder.
  • gas components easily get mixed into the target, and not only does this reduce purity, it causes abnormal electrical discharge during sputtering, induces the generation of particles, and deteriorates the deposition characteristics.
  • a Ni—Pt product formed via melting and casting has a problem in that it is extremely hard and brittle.
  • a Ni—Pt ingot is rolled, there is a problem in that grain boundary fractures occur, and it is not possible to manufacture a flat and even planar target. This is the reason targets were manufactured with the powder metallurgy process as described above.
  • Patent Document 1 considered the cause of fractures to be the coarsened crystal grains in the target and, in order to obtain fine crystal grains, attempted to inhibit the coarsening of crystals by preparing a mold with large heat capacity or a water-cooled mold, and performing rapid quenching by inhibiting the temperature rise of the mold.
  • Patent Document 1 there is a drawback in that large equipment is necessary for preparing a mold with large heat capacity or a water-cooled mold, and there is a problem in that it is difficult to inhibit the coarsening of crystals unless the cooling speed is considerably fast.
  • An object of the present invention is to provide technology capable of rolling a Ni—Pt alloy ingot upon reducing the hardness thereof, and manufacturing a rolled target stably and efficiently.
  • the present inventors discovered that by increasing the purity of the Ni—Pt alloy, it is possible to significantly reduce the hardness of the Ni—Pt alloy ingot.
  • the present invention provides 1) a Ni—Pt alloy superior in workability containing Pt in a content of 0.1 to 20 wt % and having a Vickers hardness of 40 to 90, and a target comprising the Ni—Pt alloy, and 2) the Ni—Pt alloy and Ni—Pt alloy target according to 1) above having a purity of 99.99% or higher.
  • the present invention also provides 3) a manufacturing method of Ni—Pt alloy superior in workability comprising a step of subjecting a raw material Ni having a purity of 3N level to electrochemical dissolution, a step of neutralizing the electrolytically leached solution with ammonia, a step of removing impurities by filtering the neutralized solution with activated carbon, a step of blowing carbon dioxide into the resultant solution to form nickel carbonate and exposing the resultant product to a reducing atmosphere to prepare high purity Ni powder, a step of leaching a raw material Pt having a purity of 3N level with acid, a step of subjecting the leached solution to electrolysis to prepare high purity electrodeposited Pt, and a step of dissolving the resultant high purity Ni powder and high purity electrodeposited Pt, 4) the manufacturing method of Ni—Pt alloy according to 3) above wherein the Ni—Pt alloy has a purity of 99.99% or higher, and 5) the manufacturing method of Ni—Pt alloy superior in workability according to 3) or 4)
  • the present invention also provides 6) the manufacturing method of a Ni—Pt alloy target, wherein the dissolved Ni—Pt alloy ingot manufactured based on any one of the methods according to 3) to 5) above.
  • the present invention is able to easily perform cool rolling to a dissolved Ni—Pt alloy ingot without requiring any equipment, such as preparing a mold with large heat capacity or a water-cooled mold, for accelerating the cooling speed in order to inhibit the coarsening of crystals, and yields a superior effect in that it is possible to improve the quality of the Ni—Pt alloy deposition by reducing impurities contained in the Ni—Pt alloy target and realizing high purification.
  • the present invention can be applied to a Ni—Pt alloy containing Pt in a content of 0.1 to 20 wt %.
  • This component composition is required in the deposition of a Ni—Pt alloy material of semiconductor devices, and is also a composition range of the Ni—Pt alloy or target of the present invention capable of reducing the hardness.
  • the Vickers hardness obtained by the Ni—Pt alloy of the present invention is 40 to 90.
  • the Vickers hardness is within the range of 40 to 90, and is within a range where cold rolling can be performed. This is a significant feature of the present invention.
  • the Pt content is set to be 0.1 to 20 wt %.
  • the Ni—Pt alloy and Ni—Pt alloy target of the present invention have a purity of 99.99% or higher.
  • the Vickers hardness is within the range of 40 to 90, and is within a range where cold rolling can be performed.
  • Ni—Pt alloy superior in workability is explained; as for a Ni raw material, foremost, a raw material Ni having a purity of 3N level is subject to electrochemical dissolution, the electrolytically leached solution is thereafter neutralized with ammonia, and the neutralized solution is filtered with activated carbon to remove impurities.
  • Pt raw material a raw material Pt having a purity of 3N level is leached with acid, and this leached solution is subject to electrolysis to manufacture high purity electrodeposited Pt.
  • the obtained Ni—Pt alloy has a purity of 99.99% (4N) or higher.
  • Ni—Pt alloy ingot obtained via melting and casting as described above has a Pt content of 0.1 to 20 wt % and a Vickers hardness of 40 to 90. Also as described above, this ingot is superior in workability.
  • the high purity Ni powder and high purity electrodeposited Pt obtained as described above were dissolved under a vacuum where the degree of vacuum was 10 ⁇ 4 Torr to obtain high purity Ni-20% Pt alloy.
  • the hardness of this alloy was Hv 80. This alloy was rolled at room temperature to obtain a target.
  • Example 2 As with Example 1, high purity Ni-10% Pt alloy was prepared. The hardness of this alloy was Hv 65. This alloy was rolled at room temperature to obtain a target. There were no generation of cracks or fractures in the target, and rolling could be performed easily. The results are shown in Table 2. TABLE 2 (wtppm) Example 2 Example 3 Example 4 Fe 2.0 1.9 1.8 Cr 0.6 0.6 Co 0.5 0.5 0.5 Cu 0.1 0.1 0.1 Al 0.1 0.1 0.1 O 20 20 20 C 10 10 10 N ⁇ 10 ⁇ 10 ⁇ 10 Hardness 45 55 65 Plastic Workability at Excellent Excellent Excellent Room Temperature
  • the present invention yields a superior effect in that it is easy to perform cold rolling to a dissolved Ni—Pt alloy ingot, and is capable of simultaneously reducing the impurities contained in the Ni—Pt alloy target to realize high purification. As a result, it is possible to improve the quality of Ni—Pt alloy deposition.

Abstract

The present invention provides a Ni—Pt alloy superior in workability containing Pt in a content of 0.1 to 20 wt % and having a Vickers hardness of 40 to 90, and a target comprising the Ni—Pt alloy. The present invention also provides a manufacturing method of Ni—Pt alloy superior in workability comprising a step of subjecting a raw material Ni having a purity of 3N level to electrochemical dissolution, a step of neutralizing the electrolytically leached solution with ammonia, a step of removing impurities through filtration with activated carbon, a step of blowing carbon dioxide into the resultant solution to form nickel carbonate and exposing the resultant product to a reducing atmosphere to prepare high purity Ni powder, a step of leaching a raw material Pt having a purity of 3N level with acid, a step of subjecting the leached solution to electrolysis to prepare high purity electrodeposited Pt, and a step of dissolving the resultant high purity Ni powder and high purity electrodeposited Pt. The foregoing method enables the rolling of the Ni—Pt alloy ingot upon reducing the hardness thereof, which results in the stable and efficient manufacture of a rolled target.

Description

    TECHNICAL FIELD
  • The present invention relates to a Ni—Pt alloy superior in workability, a sputtering target manufacturing by rolling a Ni—Pt alloy ingot, and a manufacturing method of such Ni—Pt alloy and Ni—Pt alloy target.
    • BACKGROUND ART
  • Ni—Pt is used as a sputtering target for semiconductor devices, and this Ni—Pt target was conventionally manufactured with the powder metallurgy process. In other words, the target was manufactured by sintering Ni powder and Pt powder, or by sintering Ni—Pt alloy powder.
  • Since it is impossible for a sintered product to become a 100% high density product, it is undeniable that such sintered product is inferior in terms of density in comparison to a target manufactured via melting, casting and rolling.
  • Therefore, gas components easily get mixed into the target, and not only does this reduce purity, it causes abnormal electrical discharge during sputtering, induces the generation of particles, and deteriorates the deposition characteristics.
  • Meanwhile, a Ni—Pt product formed via melting and casting has a problem in that it is extremely hard and brittle. As a result, when a Ni—Pt ingot is rolled, there is a problem in that grain boundary fractures occur, and it is not possible to manufacture a flat and even planar target. This is the reason targets were manufactured with the powder metallurgy process as described above.
  • In light of the foregoing circumstances, a Ni—Pt target formed via melting and casting, and which is free from cracks, has been proposed (for instance, refer to Patent Document 1).
  • This Patent Document 1 considered the cause of fractures to be the coarsened crystal grains in the target and, in order to obtain fine crystal grains, attempted to inhibit the coarsening of crystals by preparing a mold with large heat capacity or a water-cooled mold, and performing rapid quenching by inhibiting the temperature rise of the mold.
  • Nevertheless, with Patent Document 1, there is a drawback in that large equipment is necessary for preparing a mold with large heat capacity or a water-cooled mold, and there is a problem in that it is difficult to inhibit the coarsening of crystals unless the cooling speed is considerably fast.
  • Further, the crystals that come in contact with the mold are fine, and become coarse as they draw away from such mold. Thus, there is a problem in that it is difficult to obtain a uniform crystal structure, and it is therefore not possible to manufacture a target having a uniform structure or that is stable.
    • [Patent Document 1] Japanese Patent Laid-Open Publication No. S63-33563
    DISCLOSURE OF THE INVENTION
  • An object of the present invention is to provide technology capable of rolling a Ni—Pt alloy ingot upon reducing the hardness thereof, and manufacturing a rolled target stably and efficiently.
  • In order to overcome the foregoing problems, the present inventors discovered that by increasing the purity of the Ni—Pt alloy, it is possible to significantly reduce the hardness of the Ni—Pt alloy ingot.
  • Based on the foregoing discovery, the present invention provides 1) a Ni—Pt alloy superior in workability containing Pt in a content of 0.1 to 20 wt % and having a Vickers hardness of 40 to 90, and a target comprising the Ni—Pt alloy, and 2) the Ni—Pt alloy and Ni—Pt alloy target according to 1) above having a purity of 99.99% or higher.
  • Further, the present invention also provides 3) a manufacturing method of Ni—Pt alloy superior in workability comprising a step of subjecting a raw material Ni having a purity of 3N level to electrochemical dissolution, a step of neutralizing the electrolytically leached solution with ammonia, a step of removing impurities by filtering the neutralized solution with activated carbon, a step of blowing carbon dioxide into the resultant solution to form nickel carbonate and exposing the resultant product to a reducing atmosphere to prepare high purity Ni powder, a step of leaching a raw material Pt having a purity of 3N level with acid, a step of subjecting the leached solution to electrolysis to prepare high purity electrodeposited Pt, and a step of dissolving the resultant high purity Ni powder and high purity electrodeposited Pt, 4) the manufacturing method of Ni—Pt alloy according to 3) above wherein the Ni—Pt alloy has a purity of 99.99% or higher, and 5) the manufacturing method of Ni—Pt alloy superior in workability according to 3) or 4) above, wherein the Ni—Pt alloy has Pt in a content of 0.1 to 20 wt % and has a Vickers hardness of 40 to 90 Pt.
  • Further, the present invention also provides 6) the manufacturing method of a Ni—Pt alloy target, wherein the dissolved Ni—Pt alloy ingot manufactured based on any one of the methods according to 3) to 5) above.
    • EFFECT OF THE INVENTION
  • As a result, the present invention is able to easily perform cool rolling to a dissolved Ni—Pt alloy ingot without requiring any equipment, such as preparing a mold with large heat capacity or a water-cooled mold, for accelerating the cooling speed in order to inhibit the coarsening of crystals, and yields a superior effect in that it is possible to improve the quality of the Ni—Pt alloy deposition by reducing impurities contained in the Ni—Pt alloy target and realizing high purification.
  • Further, in addition to being able to prevent the generation of fractures and cracks in the target, a significant effect is yielded in that the generation of particles which often occurred in conventional sintered targets and resulted from the abnormal electrical discharge of sputtering can be inhibited.
    • BEST MODE FOR CARRYING OUT THE INVENTION
  • The present invention can be applied to a Ni—Pt alloy containing Pt in a content of 0.1 to 20 wt %. This component composition is required in the deposition of a Ni—Pt alloy material of semiconductor devices, and is also a composition range of the Ni—Pt alloy or target of the present invention capable of reducing the hardness. The Vickers hardness obtained by the Ni—Pt alloy of the present invention is 40 to 90.
  • When the Pt content contained in Ni increases, the hardness (Vickers Hv) also increases. This also has a significant influence on the amount of impurities. At 3N level, when the Pt content contained in Ni increases, the hardness increases drastically, and reaches approximately Hv 130 in the vicinity of Ni-20 wt % Pt.
  • When an ingot is rolled under this kind of circumstance where the hardness is increased, fractures arise at the grain boundary as a matter of course.
  • Meanwhile, with the high purity Ni—Pt alloy of the present invention, although the hardness gradually increases from Pt 0.1 wt % to 20 wt %, the Vickers hardness is within the range of 40 to 90, and is within a range where cold rolling can be performed. This is a significant feature of the present invention.
  • If the hardness is less than Pt 0.1 wt %, sufficient characteristics as a Ni—Pt alloy cannot be obtained, and if the hardness exceeds Pt 20 wt %, as described above, the target becomes too hard and difficult to process. Thus, the Pt content is set to be 0.1 to 20 wt %.
  • As a result, in addition to being able to prevent the generation of fractures and cracks in the target, a significant effect is yielded in that the generation of particles which often occurred in conventional sintered targets and resulted from the abnormal electrical discharge of sputtering can be inhibited.
  • The Ni—Pt alloy and Ni—Pt alloy target of the present invention have a purity of 99.99% or higher. As a result, the Vickers hardness is within the range of 40 to 90, and is within a range where cold rolling can be performed.
  • The manufacturing method of this kind of Ni—Pt alloy superior in workability is explained; as for a Ni raw material, foremost, a raw material Ni having a purity of 3N level is subject to electrochemical dissolution, the electrolytically leached solution is thereafter neutralized with ammonia, and the neutralized solution is filtered with activated carbon to remove impurities.
  • Next, carbon dioxide is blown into this resultant solution to obtain nickel carbonate, and this is subject to reducing atmosphere to manufacture high purity Ni powder.
  • Meanwhile, as for Pt raw material, a raw material Pt having a purity of 3N level is leached with acid, and this leached solution is subject to electrolysis to manufacture high purity electrodeposited Pt.
  • Next, the high purity Ni powder and high purity electrodeposited Pt obtained above are dissolved. The obtained Ni—Pt alloy has a purity of 99.99% (4N) or higher.
  • Further, the Ni—Pt alloy ingot obtained via melting and casting as described above has a Pt content of 0.1 to 20 wt % and a Vickers hardness of 40 to 90. Also as described above, this ingot is superior in workability.
  • As a result of performing cold rolling to this dissolved Ni—Pt alloy ingot manufactured as described above, it is possible to easily manufacture a Ni—Pt alloy target.
  • Thus, in addition to being able to prevent the generation of fractures and cracks in the target, a significant effect is yielded in that the generation of particles which often occurred in conventional sintered targets and resulted from the abnormal electrical discharge of sputtering can be inhibited.
    • EXAMPLES
  • Examples of the present invention are now explained. These Examples are merely illustrative, and the present invention shall in no way be limited thereby. In other words, the present invention shall only be limited by the scope of the present invention, and shall include the various modifications other than the Examples of this invention.
    • Example 1
  • 10 kg of 3N level Ni raw material shown in Table 1 was used as the anode, and this was subject to electrolytic leaching with hydrochloric acid solution. At the point when it became 100 g/L, the resultant solution was neutralized with ammonia, and pH was set to 8. This resultant solution was filtered by adding 10 g/L of activated carbon to remove impurities.
  • Next, carbon dioxide was blown into this resultant solution to obtain nickel carbonate. The resultant solution was subject to heat treatment at a temperature of 1200° C. under H2 atmosphere to obtain 8 kg of high purity Ni powder.
  • Meanwhile, 5 kg of 3N level Pt was used and dissolved in royal water. The resultant solution was made to be a pH 2 level, and this was subject to electrolytic winning to obtain high purity electrodeposited Pt. Carbon was used as the anode during electrolytic winning.
  • The high purity Ni powder and high purity electrodeposited Pt obtained as described above were dissolved under a vacuum where the degree of vacuum was 10−4 Torr to obtain high purity Ni-20% Pt alloy. The hardness of this alloy was Hv 80. This alloy was rolled at room temperature to obtain a target.
  • There were no generation of cracks or fractures in the target, and rolling could be performed easily. The results are shown in Table 1.
    TABLE 1
    (wtppm)
    Compar-
    Raw Raw High High Exam- ative
    Material Material Purity Purity ple Example
    Ni Pt Ni Pt 1 1
    Fe 110 10 2.1 1.0 1.7 90
    Cr 50 2 0.6 0.5 0.6 44
    Co 60 5 0.5 0.2 0.4 49
    Cu 30 4 0.1 0.1 0.1 25
    Al 10 8 0.1 0.1 0.1 9.5
    O 150 70 20 <10 10 130
    C 80 20 10 <10 10 70
    N 30 10 <10 <10 <10 25
    Hardness 100 40 70 30 80 110
    Plastic Fair Good Good Excel- Excel- Infe-
    Workability lent lent rior
    at Room
    Temperature
    • Example 2
  • As with Example 1, high purity Ni-0.5% Pt alloy was prepared. The hardness of this alloy was Hv 45. This alloy was rolled at room temperature to obtain a target. There were no generation of cracks or fractures in the target, and rolling could be performed easily. The results are shown in Table 2.
    • Example 3
  • As with Example 1, high purity Ni-5% Pt alloy was prepared. The hardness of this alloy was Hv 55. This alloy was rolled at room temperature to obtain a target. There were no generation of cracks or fractures in the target, and rolling could be performed easily. The results are shown in Table 2.
    • Example 4
  • As with Example 1, high purity Ni-10% Pt alloy was prepared. The hardness of this alloy was Hv 65. This alloy was rolled at room temperature to obtain a target. There were no generation of cracks or fractures in the target, and rolling could be performed easily. The results are shown in Table 2.
    TABLE 2
    (wtppm)
    Example 2 Example 3 Example 4
    Fe 2.0 1.9 1.8
    Cr 0.6 0.6 0.6
    Co 0.5 0.5 0.5
    Cu 0.1 0.1 0.1
    Al 0.1 0.1 0.1
    O 20 20 20
    C 10 10 10
    N <10 <10 <10
    Hardness 45 55 65
    Plastic Workability at Excellent Excellent Excellent
    Room Temperature
    • Comparative Example 1
  • Pt having the same purity as 3N level Ni was dissolved to become Ni-20 wt %. As a result, the hardness of the obtained ingot was Hv 110. This ingot was extremely hard, and plastic working at room temperature was difficult. The results are shown in Table 1 in comparison to Example 1.
    • INDUSTRIAL APPLICABILITY
  • As described above, the present invention yields a superior effect in that it is easy to perform cold rolling to a dissolved Ni—Pt alloy ingot, and is capable of simultaneously reducing the impurities contained in the Ni—Pt alloy target to realize high purification. As a result, it is possible to improve the quality of Ni—Pt alloy deposition.
  • Further, in addition to being able to prevent the generation of fractures and cracks in the target, a significant effect is yielded in that the generation of particles resulting from the abnormal electrical discharge of sputtering can be inhibited. Therefore, this is suitable for the deposition of Ni—Pt alloy in a semiconductor device.

Claims (12)

1. A Ni—Pt alloy superior in workability containing Pt in a content of 0.1 to 20 wt % and having a Vickers hardness of 40 to 90.
2. The Ni—Pt alloy according to claim 1 having a purity of 99.99% or higher.
3. A method of manufacturing Ni—Pt alloy superior in workability, comprising the steps of:
subjecting a raw material Ni having a purity of 3N level to electrochemical dissolution,
neutralizing the electrolytically leached solution with ammonia,
removing impurities by filtering the neutralized solution with activated carbon,
blowing carbon dioxide into the resultant solution to form nickel carbonate and exposing the resultant product to a reducing atmosphere to prepare high purity Ni powder,
leaching a raw material Pt having a purity of 3N level with acid,
subjecting the leached solution to electrolysis to prepare high purity electrodeposited Pt, and
dissolving the resultant high purity Ni powder and high purity electrodeposited Pt.
4. The method according to claim 3, wherein the Ni—Pt alloy has a purity of 99.99% or higher.
5-6. (canceled)
7. A Ni—Pt alloy target superior in workability containing Pt in a content of 0.1 to 20 wt % and having a Vickers hardness of 40 to 90.
8. The Ni—Pt alloy target according to claim 7 having a purity of 99.99% or higher.
9. A method according to claim 4, wherein the Ni—Pt alloy has Pt in a content of 0.1 to 20 wt % and has a Vickers hardness of 40 to 90.
10. A method according to claim 9, further comprising the step of manufacturing a Ni—Pt alloy sputtering target from the high purity Ni powder and high purity electrodeposited Pt after said dissolving step.
11. A method according to claim 3, wherein the Ni—Pt alloy has Pt in a content of 0. 1 to 20 wt % and has a Vickers hardness of 40 to 90.
12. A method according to claim 11, further comprising the step of manufacturing a Ni—Pt alloy sputtering target from the high purity Ni powder and high purity electrodeposited Pt after said dissolving step.
13. A method according to claim 3, further comprising the step of manufacturing a Ni—Pt alloy sputtering target from the high purity Ni powder and high purity electrodeposited Pt after said dissolving step.
US10/596,671 2004-03-01 2005-02-08 Ni-pt alloy and target comprising the alloy Abandoned US20070098590A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US12/957,013 US7959782B2 (en) 2004-03-01 2010-11-30 Method of manufacturing a Ni-Pt alloy

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2004056097 2004-03-01
JP2004-056097 2004-03-01
PCT/JP2005/001813 WO2005083138A1 (en) 2004-03-01 2005-02-08 Ni-Pt ALLOY AND TARGET COMPRISING THE ALLOY

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2005/001813 A-371-Of-International WO2005083138A1 (en) 2004-03-01 2005-02-08 Ni-Pt ALLOY AND TARGET COMPRISING THE ALLOY

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US12/957,013 Division US7959782B2 (en) 2004-03-01 2010-11-30 Method of manufacturing a Ni-Pt alloy

Publications (1)

Publication Number Publication Date
US20070098590A1 true US20070098590A1 (en) 2007-05-03

Family

ID=34908895

Family Applications (2)

Application Number Title Priority Date Filing Date
US10/596,671 Abandoned US20070098590A1 (en) 2004-03-01 2005-02-08 Ni-pt alloy and target comprising the alloy
US12/957,013 Active US7959782B2 (en) 2004-03-01 2010-11-30 Method of manufacturing a Ni-Pt alloy

Family Applications After (1)

Application Number Title Priority Date Filing Date
US12/957,013 Active US7959782B2 (en) 2004-03-01 2010-11-30 Method of manufacturing a Ni-Pt alloy

Country Status (7)

Country Link
US (2) US20070098590A1 (en)
EP (2) EP2468906B1 (en)
JP (2) JP4409572B2 (en)
KR (2) KR100925691B1 (en)
CN (1) CN100567535C (en)
TW (1) TWI264480B (en)
WO (1) WO2005083138A1 (en)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040256035A1 (en) * 2002-01-18 2004-12-23 Yasuhiro Yamakoshi Target of high-purity nickel or nickel alloy and its producing method
US20060037680A1 (en) * 2003-01-10 2006-02-23 Nikko Materials Co., Ltd Nickel alloy sputtering target
US20060292028A1 (en) * 2003-10-07 2006-12-28 Nikko Materials Co., Ltd. High-purity ni-v alloy target therefrom high-purity ni-v alloy thin film and process for producing high-purity ni-v alloy
US20070074790A1 (en) * 2003-10-24 2007-04-05 Nikko Materials Co., Ltd. Nickel alloy sputtering target and nickel alloy thin film
US20090028744A1 (en) * 2007-07-23 2009-01-29 Heraeus, Inc. Ultra-high purity NiPt alloys and sputtering targets comprising same
WO2010080469A2 (en) 2008-12-19 2010-07-15 E. I. Du Pont De Nemours And Company Mechanically reliable solar cell modules
US20110068014A1 (en) * 2004-03-01 2011-03-24 Jx Nippon Mining & Metals Corporation Ni-Pt Alloy and Target Comprising the Same
US20110135942A1 (en) * 2009-02-10 2011-06-09 Jx Nippon Mining & Metals Corporation Nickel Alloy Sputtering Target and Nickel Silicide Film
US9249497B2 (en) 2010-03-19 2016-02-02 Jx Nippon Mining & Metals Corporation Ni alloy sputtering target, Ni alloy thin film and Ni silicide film
US9328412B2 (en) 2010-08-31 2016-05-03 Jx Nippon Mining & Metals Corporation Fe—Pt-based ferromagnetic material sputtering target
US10337100B2 (en) 2014-03-27 2019-07-02 Jx Nippon Mining & Metals Corporation Sputtering target comprising Ni—P alloy or Ni—Pt—P alloy and production method therefor
CN113881920A (en) * 2020-07-03 2022-01-04 光洋应用材料科技股份有限公司 Nickel-platinum alloy target material and manufacturing method thereof

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009119196A1 (en) * 2008-03-28 2009-10-01 日鉱金属株式会社 Platinum powder for magnetic material target, method for producing the powder, method for producing magnetic material target composed of platinum sintered compact, and the sintered magnetic material target
KR101032011B1 (en) 2009-02-10 2011-05-02 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 Nickel Alloy Sputtering Targets and Nickel Silicide Films
US8968537B2 (en) * 2011-02-09 2015-03-03 Applied Materials, Inc. PVD sputtering target with a protected backing plate
JP6340621B2 (en) * 2013-07-26 2018-06-13 三菱マテリアル株式会社 Ni sputtering target and manufacturing method thereof
CN104726829A (en) * 2013-12-18 2015-06-24 有研亿金新材料股份有限公司 High purity NiPt alloy target material and preparation method thereof
CN104018128B (en) * 2014-05-29 2016-08-24 贵研铂业股份有限公司 A kind of nickel platinum alloy sputtering target material and preparation method thereof
WO2015183600A1 (en) 2014-05-30 2015-12-03 National Oilwell Varco, L.P. Wellsite pump with integrated driver and hydraulic motor and method of using same
TWI612146B (en) 2015-06-26 2018-01-21 國立大學法人東京工業大學 Silicide alloy film for semiconductor device electrode and method for manufacturing silicide alloy film
CN106282639B (en) * 2016-09-19 2018-02-16 中材科技股份有限公司 A kind of platinum-nickel alloy sputtering target material and preparation method thereof
CN111304608B (en) * 2020-03-17 2021-10-15 贵研铂业股份有限公司 Nickel-platinum alloy sputtering target with high oriented crystal grains and preparation method thereof
CN112853131B (en) * 2020-12-30 2022-07-19 有研亿金新材料有限公司 Preparation method of high-purity low-gas-content nickel-platinum alloy
IT202100003281A1 (en) 2021-02-15 2022-08-15 Bluclad S P A HYPOALLERGENIC ELECTRODEPOSITED PT-NI ALLOY AND RELATED BATH AND GALVANIC CYCLE

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2269497A (en) * 1940-08-26 1942-01-13 Owens Corning Flberglas Corp Nickel-platinum alloy
US5188713A (en) * 1991-03-05 1993-02-23 Envirochip Technologies Ltd. Process for recovery of metal
US5282946A (en) * 1991-08-30 1994-02-01 Mitsubishi Materials Corporation Platinum-cobalt alloy sputtering target and method for manufacturing same
US6238494B1 (en) * 1997-07-11 2001-05-29 Johnson Matthey Electronics Inc. Polycrystalline, metallic sputtering target
US6531396B1 (en) * 1999-11-17 2003-03-11 Institute Of Materials Research And Engineering Method of fabricating a nickel/platinum monsilicide film
US20040256035A1 (en) * 2002-01-18 2004-12-23 Yasuhiro Yamakoshi Target of high-purity nickel or nickel alloy and its producing method
US20060037680A1 (en) * 2003-01-10 2006-02-23 Nikko Materials Co., Ltd Nickel alloy sputtering target

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6333563A (en) * 1986-07-25 1988-02-13 Tanaka Kikinzoku Kogyo Kk Production of pt-ni alloy for sputtering
GB2242203A (en) 1990-03-21 1991-09-25 Johnson Matthey Plc Catalyst material comprising platinum alloy supported on carbon
JPH0543921A (en) * 1991-08-12 1993-02-23 Murata Mfg Co Ltd Production of nickel fine powder
JPH11152592A (en) * 1997-11-18 1999-06-08 Japan Energy Corp Production of high purity nickel and high purity nickel material for forming thin film
JPH11335821A (en) 1998-05-20 1999-12-07 Japan Energy Corp Nickel-iron alloy sputtering target for forming magnetic thin film, production of magnetic thin film and nickel-iron alloy sputtering target for forming magnetic thin film
US20020139457A1 (en) * 2001-04-02 2002-10-03 Coppola Vito A. Method of suppressing the oxidation characteristics of nickel
EP1413651A4 (en) 2001-08-01 2006-10-25 Nippon Mining Co Method for producing high purity nickel, high purity nickel, sputtering target comprising the high purity nickel, and thin film formed by using said spattering target
JP2003213405A (en) * 2002-01-18 2003-07-30 Nikko Materials Co Ltd High purity nickel or nickel alloy target and production method therefor
JP2003213407A (en) * 2002-01-24 2003-07-30 Nikko Materials Co Ltd High purity nickel or nickel alloy sputtering target and production method therefor
US6845542B2 (en) * 2002-08-27 2005-01-25 The Research Foundation Of State University Of New York Portable, fully contained and disposable suction device
JP4447556B2 (en) 2003-10-07 2010-04-07 日鉱金属株式会社 High purity Ni-V alloy, target made of the same Ni-V alloy, Ni-V alloy thin film, and method for producing high purity Ni-V alloy
JP4271684B2 (en) 2003-10-24 2009-06-03 日鉱金属株式会社 Nickel alloy sputtering target and nickel alloy thin film
US20070098590A1 (en) 2004-03-01 2007-05-03 Nikko Materials Co., Ltd. Ni-pt alloy and target comprising the alloy

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2269497A (en) * 1940-08-26 1942-01-13 Owens Corning Flberglas Corp Nickel-platinum alloy
US5188713A (en) * 1991-03-05 1993-02-23 Envirochip Technologies Ltd. Process for recovery of metal
US5282946A (en) * 1991-08-30 1994-02-01 Mitsubishi Materials Corporation Platinum-cobalt alloy sputtering target and method for manufacturing same
US6238494B1 (en) * 1997-07-11 2001-05-29 Johnson Matthey Electronics Inc. Polycrystalline, metallic sputtering target
US6531396B1 (en) * 1999-11-17 2003-03-11 Institute Of Materials Research And Engineering Method of fabricating a nickel/platinum monsilicide film
US20040256035A1 (en) * 2002-01-18 2004-12-23 Yasuhiro Yamakoshi Target of high-purity nickel or nickel alloy and its producing method
US20060037680A1 (en) * 2003-01-10 2006-02-23 Nikko Materials Co., Ltd Nickel alloy sputtering target

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040256035A1 (en) * 2002-01-18 2004-12-23 Yasuhiro Yamakoshi Target of high-purity nickel or nickel alloy and its producing method
US20060137782A1 (en) * 2002-01-18 2006-06-29 Nikko Materials Co., Ltd. Target of high-purity nickel or nickel alloy and its producing method
US7740718B2 (en) 2002-01-18 2010-06-22 Nippon Mining & Metals Co., Ltd. Target of high-purity nickel or nickel alloy and its producing method
US7618505B2 (en) 2002-01-18 2009-11-17 Nippon Mining & Metals Co., Ltd. Target of high-purity nickel or nickel alloy and its producing method
US20060037680A1 (en) * 2003-01-10 2006-02-23 Nikko Materials Co., Ltd Nickel alloy sputtering target
US8871144B2 (en) 2003-10-07 2014-10-28 Jx Nippon Mining & Metals Corporation High-purity Ni-V alloy target therefrom high-purity Ni-V alloy thin film and process for producing high-purity Ni-V alloy
US20060292028A1 (en) * 2003-10-07 2006-12-28 Nikko Materials Co., Ltd. High-purity ni-v alloy target therefrom high-purity ni-v alloy thin film and process for producing high-purity ni-v alloy
US20100242674A1 (en) * 2003-10-07 2010-09-30 Nippon Mining And Metals Co., Ltd. High-Purity Ni-V Alloy, Target therefrom, High-Purity Ni-V Alloy Thin Film and Process for Producing High-Purity Ni-V Alloy
US7938918B2 (en) 2003-10-07 2011-05-10 Jx Nippon Mining & Metals Corporation High-purity Ni-V alloy, target therefrom, high-purity Ni-V alloy thin film and process for producing high-purity Ni-V alloy
US7605481B2 (en) 2003-10-24 2009-10-20 Nippon Mining & Metals Co., Ltd. Nickel alloy sputtering target and nickel alloy thin film
US20070074790A1 (en) * 2003-10-24 2007-04-05 Nikko Materials Co., Ltd. Nickel alloy sputtering target and nickel alloy thin film
US7959782B2 (en) 2004-03-01 2011-06-14 Jx Nippon Mining & Metals Corporation Method of manufacturing a Ni-Pt alloy
US20110068014A1 (en) * 2004-03-01 2011-03-24 Jx Nippon Mining & Metals Corporation Ni-Pt Alloy and Target Comprising the Same
US20090028744A1 (en) * 2007-07-23 2009-01-29 Heraeus, Inc. Ultra-high purity NiPt alloys and sputtering targets comprising same
WO2010080469A2 (en) 2008-12-19 2010-07-15 E. I. Du Pont De Nemours And Company Mechanically reliable solar cell modules
US20110135942A1 (en) * 2009-02-10 2011-06-09 Jx Nippon Mining & Metals Corporation Nickel Alloy Sputtering Target and Nickel Silicide Film
CN102165094A (en) * 2009-02-10 2011-08-24 Jx日矿日石金属株式会社 Nickel alloy sputtering target and nickel silicide film
US8114341B2 (en) 2009-02-10 2012-02-14 Jx Nippon Mining & Metals Corporation Nickel alloy sputtering target and nickel silicide film
US9249497B2 (en) 2010-03-19 2016-02-02 Jx Nippon Mining & Metals Corporation Ni alloy sputtering target, Ni alloy thin film and Ni silicide film
US9328412B2 (en) 2010-08-31 2016-05-03 Jx Nippon Mining & Metals Corporation Fe—Pt-based ferromagnetic material sputtering target
US10337100B2 (en) 2014-03-27 2019-07-02 Jx Nippon Mining & Metals Corporation Sputtering target comprising Ni—P alloy or Ni—Pt—P alloy and production method therefor
CN113881920A (en) * 2020-07-03 2022-01-04 光洋应用材料科技股份有限公司 Nickel-platinum alloy target material and manufacturing method thereof

Also Published As

Publication number Publication date
JP5113134B2 (en) 2013-01-09
JPWO2005083138A1 (en) 2007-11-22
EP1721997B1 (en) 2012-03-28
CN1926254A (en) 2007-03-07
US7959782B2 (en) 2011-06-14
KR101021488B1 (en) 2011-03-16
KR100925691B1 (en) 2009-11-10
JP2010047843A (en) 2010-03-04
US20110068014A1 (en) 2011-03-24
EP2468906A1 (en) 2012-06-27
EP1721997A4 (en) 2009-11-11
WO2005083138A1 (en) 2005-09-09
CN100567535C (en) 2009-12-09
JP4409572B2 (en) 2010-02-03
EP2468906B1 (en) 2014-07-23
TW200530429A (en) 2005-09-16
EP1721997A1 (en) 2006-11-15
KR20090101393A (en) 2009-09-25
TWI264480B (en) 2006-10-21
KR20060114384A (en) 2006-11-06

Similar Documents

Publication Publication Date Title
US7959782B2 (en) Method of manufacturing a Ni-Pt alloy
US8216442B2 (en) Ultrahigh-purity copper and process for producing the same
KR100997560B1 (en) Copper alloy with high strength and excellent processability in bending and process for producing copper alloy sheet
US10266924B2 (en) Tantalum sputtering target
KR102327963B1 (en) High purity copper sputtering target material
WO2006132317A1 (en) Copper alloy, copper alloy plate, and process for producing the same
JP2008031525A (en) Copper alloy having high strength and high softening resistance
EP2604718B1 (en) Tantalum sputtering target
US20160217983A1 (en) Tantalum sputtering target
US20150232980A1 (en) Cu-Ga Alloy Sputtering Target, and Method for Producing Same
EP2692877A1 (en) Copper alloy and method for producing copper alloy
JP2019183256A (en) Sputtering target material
CN112375939A (en) Cu-Ni-Zr-V-B copper alloy material and preparation method thereof
JP4904455B2 (en) Copper alloy and manufacturing method thereof
KR101560455B1 (en) LCD Glass METHOD OF MANUFACTURING AN OXIDE DISPERSION STRENGTHENED PLATINUMRHODIUM ALLOYS MATERIALS USING SPARK PLASMA SINTERING FOR LIQUID CRYSTAL DISPLAY GLASS MANUFACTURING
CN115821171B (en) Trace B element doped modified high-strength high-plasticity multicomponent alloy, and preparation method and application thereof
JP4133688B2 (en) Copper alloy with high strength and high bending workability
KR20210111671A (en) sputtering target material
JP2003138322A (en) Method of manufacturing high-purity metal, high-purity metal, sputtering target consisting of this high-purity metal and thin film formed by this sputtering target
JP2010202914A (en) Method for producing cobalt excellent in acid solubility

Legal Events

Date Code Title Description
AS Assignment

Owner name: NIKKO MATERIALS CO., LTD., JAPAN

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:SHINDO, YUICHIRO;REEL/FRAME:018012/0573

Effective date: 20060605

AS Assignment

Owner name: NIPPON MINING & METALS CO., LTD.,JAPAN

Free format text: CHANGE OF NAME;ASSIGNOR:NIKKO MATERIALS CO., LTD.;REEL/FRAME:018560/0126

Effective date: 20060403

Owner name: NIPPON MINING & METALS CO., LTD., JAPAN

Free format text: CHANGE OF NAME;ASSIGNOR:NIKKO MATERIALS CO., LTD.;REEL/FRAME:018560/0126

Effective date: 20060403

AS Assignment

Owner name: NIPPON MINING HOLDINGS, INC., JAPAN

Free format text: MERGER;ASSIGNOR:NIPPON MINING & METALS CO., LTD.;REEL/FRAME:025115/0062

Effective date: 20100701

AS Assignment

Owner name: JX NIPPON MINING & METALS CORPORATION, JAPAN

Free format text: CHANGE OF NAME;ASSIGNOR:NIPPON MINING HOLDINGS, INC.;REEL/FRAME:025123/0358

Effective date: 20100701

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION