US20110162322A1 - Method for Storing Target Comprising Rare Earth Metal or Oxide Thereof - Google Patents

Method for Storing Target Comprising Rare Earth Metal or Oxide Thereof Download PDF

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Publication number
US20110162322A1
US20110162322A1 US13/119,377 US200913119377A US2011162322A1 US 20110162322 A1 US20110162322 A1 US 20110162322A1 US 200913119377 A US200913119377 A US 200913119377A US 2011162322 A1 US2011162322 A1 US 2011162322A1
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Prior art keywords
target
oxide
rare earth
earth metal
storing
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US13/119,377
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English (en)
Inventor
Kazuyuki Satoh
Yoshimasa Koido
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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Assigned to JX NIPPON MINING & METALS CORPORATION reassignment JX NIPPON MINING & METALS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KOIDO, YOSHIMASA, SATOH, KAZUYUKI
Publication of US20110162322A1 publication Critical patent/US20110162322A1/en
Abandoned legal-status Critical Current

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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
    • B65D81/24—Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
    • B65D81/26—Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants with provision for draining away, or absorbing, or removing by ventilation, fluids, e.g. exuded by contents; Applications of corrosion inhibitors or desiccators
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F15/00—Other methods of preventing corrosion or incrustation

Definitions

  • the present invention relates to a method for storing a target comprising a rare earth metal or oxide thereof that is easily pulverized due to oxidation or hydroxylation.
  • Rare earth metals are contained in the earth's crust as a mixed composite oxide. Rare-earth elements are so called because they are separated from relatively rare minerals, but they are not that rare in light of the overall earth's crust. In recent years, rare earth metals are attracting attention as an electronic material, and research and development for using rare earth metals are being promoted.
  • lanthanum is a white metal having an atomic number of 57 and an atomic weight of 138.9, and comprises a double hexagonal close-packed structure at normal temperature.
  • Lanthanum has a melting point of 921° C., boiling point of 3500° C., and density of 6.15 g/cm 3 , its surface is oxidized in the atmosphere, and it gradually melts in water.
  • Lanthanum is a metal that is attracting attention as an electronic material such as a metal gate material or a high-dielectric constant (High-k) material. Rare earth elements other than lanthanum also have attributes similar to lanthanum.
  • a rare earth metal such as lanthanum is a material in which high purification is difficult to achieve since it is easily oxidized during the refining process.
  • a rare earth metal such as lanthanum is left in the atmosphere, there is a problem in that the handling thereof is difficult since it will become oxidized and tarnished in a short time.
  • rare earth metals such as lanthanum and their oxides are still in the research phase.
  • a rare earth metal or oxide thereof itself exists as a sputtering target material, it is possible to form a thin film of such rare earth metal or oxide thereof on a substrate. It will be easy to study the behavior at the interface with the silicon substrate, and the properties of a high-dielectric gate insulator film or the like after forming a rare earth metal compound. There is also a significant advantage in that the freedom of the target as a product will increase.
  • a lanthanum sputtering target is prepared, as described above, it becomes oxidized in a short time in the atmosphere.
  • a stable oxide layer is formed on a metal target surface, but since it is extremely thin, it peels off during the initial stage of sputtering and does not affect the sputtering characteristics significantly.
  • the oxide layer becomes thick, and deterioration of the electrical conductivity will occur and thereby cause defective sputtering.
  • the lanthanum sputtering target is left in the atmosphere for a long time, it reacts with the moisture in the air to become covered with white hydroxide powder and ultimately become pulverized, and it may even cause a problem of not allowing normal sputtering to be performed.
  • the target is prepared, it is necessary to take measures for preventing oxidation and hydroxylation such as by immediately vacuum-packing or coating the target with fats and oils.
  • the standard method is to store the rare earth metals in mineral oil in order to prevent such rare earth metals from being exposed to the air.
  • it is necessary to clean the target before its use in order to remove the mineral oil.
  • the cleaning of the target itself is difficult due to its reactivity with oxygen, moisture and carbon dioxide.
  • Patent Document 1 International Publication No. W02005/037649
  • Patent Document 2 Japanese Laid-Open Patent Publication No. 2002-212718
  • Patent Document 3 Japanese Laid-Open Patent Publication No. 2001-240959
  • Patent Document 4 Japanese Laid-Open Patent Publication No. H8-246135
  • Patent Document 5 Japanese Laid-Open Patent Publication No. H4-231461
  • An object of this invention is to provide technology for allowing the long-term storage of a sputtering target in enabled condition by devising the method for storing a target comprising a rare earth metal or oxide thereof, and thereby inhibiting the pulverization of the target caused by the oxidation and hydroxylation of such target due to residual air or ingress of air.
  • the present invention provides:
  • the present invention additionally provides:
  • the present invention further provides:
  • FIG. 1 A diagram showing an example where the surface and side face of the La target are thinly coated with La oxide powder and vacuum packing is performed thereto.
  • FIG. 2 A diagram showing an example where La oxide powder is placed in a space due to the unevenness (difference in level) between the La target and BP (backing plate) and vacuum packing is performed thereto.
  • FIG. 3 A diagram showing an example where a La target is placed in a metallic container, La oxide powder is filled around the periphery of the La target, ambient air is once replaced with argon having a dew point of ⁇ 80° C. or less, and vacuum sealing is subsequently performed thereto.
  • FIG. 4 A diagram showing an example where a metal alloy target comprising La and Er is placed in a metallic container, a sintered La oxide block is placed at the uneven part between the target and BP, air in the container is replaced with argon gas, and vacuuming is subsequently performed thereto.
  • FIG. 5 A diagram showing an example where the La target is subject to vacuum sealing with a film.
  • FIG. 6 A diagram showing an example where the La target is subject to vacuum sealing with a film, and silica gel is placed as a desiccant.
  • FIG. 7 A diagram showing an example where the La 2 O 3 target is subject to vacuum sealing with a film.
  • Rare earths in particular lanthanum and lanthanum oxide, are known to have extremely strong hygroscopic properties (reactivity with moisture).
  • the challenge to date was how to prevent lanthanum and lanthanum oxide from absorbing moisture as much as possible, and how to store lanthanum and lanthanum oxide in an environment with minimal moisture.
  • the oxidation or hydroxylation of the lanthanum target body can be prevented by coating, mounting or placing lanthanum oxide (powder or sintered compact of a plate or block) on the target surface upon storing the lanthanum target.
  • moisture when storing a lanthanum oxide target, moisture can be absorbed and eliminated more effectively by enclosing the powdered or granular lanthanum oxide of larger surface area and, therefore, degradation of the target caused by hydroxylation can be prevented.
  • the method for storing a target comprising a rare earth metal or oxide thereof according to the present invention is to introduce, as a desiccant, oxide of the same rare earth metal as the material of the rare earth metal or its oxide target to be stored into a storage container or a film-type seal.
  • an oxide of the rare earth metal with the greatest hygroscopic property can be used as a desiccant.
  • encapsulating and storing method for target it is preferable to prevent the ingress of outside air as much as possible. Vacuum sealing can be performed as one such method. Moreover, when vacuum sealing and storing the target, it is preferable to once replace the inside of the container or the film-type seal with inert gas having a dew point of ⁇ 80° C. or less and thereafter perform vacuum sealing.
  • flexible film may be used in the form of a hermetic bag and subject to vacuum sealing.
  • inert gas having a dew point of ⁇ 80° C. or less may be filled and sealed as the method for storing a target. All of the foregoing methods prevent the ingress of outside air.
  • a target is generally bonded to a backing plate.
  • a flexible film in the form of a hermetic bag and performing vacuum sealing thereto, unevenness will inevitably arise between the target and the backing plate, and a space is likely to be formed. Outside air is easily accumulated in such space. Pulverization of the target tends to advance from such space.
  • the rare earth oxide to be used as the desiccant is preferably in the form of powder or granule of large surface area. Nevertheless, it is effective to simply place a small piece of rare earth oxide at a location where outside air is easily accumulated.
  • the method for storing a target according to the present invention is particularly effective for a lanthanum target or a target containing lanthanum as the rare earth metal configuring the target.
  • the foregoing rare earth oxide to be used as the desiccant is lanthanum oxide. This is ironic, but lanthanum oxide that is most easily hydroxylated has the greatest inhibitory effect on hydroxylation of a target comprising a rare earth metal or oxide thereof in the method for storing a target comprising a rare earth metal or oxide thereof.
  • Table 1 shows the favorable examples of the flexible film to be used in encapsulating and storing the target, as well as the non-favorable examples.
  • Table 1 the examples having properties of GX Barrier (product name) or higher are effective. As shown in Table 1, GX Barrier (product name) and a bag containing Al foil are favorable. Table 1 shows representative examples, and it goes without saying that other flexible films may be used so as long as they satisfy the foregoing conditions.
  • the lanthanum oxide powder absorbs the moisture remaining inside the vacuum package and the moisture that penetrates the film and is fixed as lanthanum hydroxide.
  • this is effective in preventing the phenomenon where the La target surface reacts with moisture to become hydroxide and be pulverized.
  • lanthanum oxide absorbs the moisture remaining after the vacuuming and is fixed as lanthanum hydroxide.
  • this is effective in preventing the phenomenon where La reacts with moisture to become hydroxide and be pulverized.
  • lanthanum oxide absorbs the moisture remaining after the vacuuming and is fixed as lanthanum hydroxide.
  • this is effective in preventing the phenomenon where La reacts with moisture to become hydroxide and be pulverized.
  • FIG. 5 This is an example where the La target was subject to vacuum sealing with a film.
  • FIG. 5 A specific example is shown in FIG. 5 .
  • the small amount of moisture remaining in the space created between the vacuum-packing film and the target reacted with the La target, and La became lanthanum hydroxide. It resulted in pulverization.
  • silica gel When silica gel is placed as shown in FIG. 6 , pulverization progressed faster than the case of not placing silica gel. The reason for this is considered to be that the moisture adsorbed by the silica gel became desorbed and discharged inside the vacuum-packing film, and the reaction of moisture and La was promoted and resulted in lanthanum hydroxide. In light of the above, it is evident that silica gel that is used as a general desiccant is useless, or even undesirable, in preventing the pulverization phenomenon of the rare earth metal or rare earth metal oxide.
  • the method for storing a target comprising a rare earth metal or oxide thereof according to the present invention is to introduce, as a desiccant, oxide of the same rare earth metal as the material of the target comprising the rare earth metal or oxide thereof to be stored into a storage container or a film-type seal. It is thereby possible to effectively inhibit the condition where the target reacts with the moisture in the atmosphere and becomes covered with white hydroxide powder.
  • targets can be stably supplied as an electronic material such as a metal gate material or a high-dielectric constant (High-k) material, and the present invention is extremely useful industrially.
  • an electronic material such as a metal gate material or a high-dielectric constant (High-k) material

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Food Science & Technology (AREA)
  • Physical Vapour Deposition (AREA)
  • Packages (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
US13/119,377 2008-10-29 2009-10-23 Method for Storing Target Comprising Rare Earth Metal or Oxide Thereof Abandoned US20110162322A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2008277725 2008-10-29
JP2008-277725 2008-10-29
PCT/JP2009/068248 WO2010050409A1 (ja) 2008-10-29 2009-10-23 希土類金属又はこれらの酸化物からなるターゲットの保管方法

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US (1) US20110162322A1 (zh)
JP (1) JP5032662B2 (zh)
KR (1) KR101290941B1 (zh)
CN (1) CN102203314B (zh)
TW (1) TWI472458B (zh)
WO (1) WO2010050409A1 (zh)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100272596A1 (en) * 2007-12-28 2010-10-28 Nippon Mining And Metals Co., Ltd. High-Purity Lanthanum, Sputtering Target Comprising High-Purity Lanthanum, and Metal Gate Film Mainly Comprising High-Purity Lanthanum
US20110114481A1 (en) * 2008-07-07 2011-05-19 Jx Nippon Mining & Metals Corporation Lanthanum Oxide-based Sintered Compact, Sputtering Target Composed of said Sintered Compact, Method of Producing Lanthanum Oxide-based Sintered Compact, and Method of Producing Sputtering Target based on said Production Method
US20110114482A1 (en) * 2008-07-07 2011-05-19 Jx Nippon Mining & Metals Corporation Oxide Sintered Compact, Sputtering Target Composed of the Sintered Compact, and Method of Producing the Sintered Compact and the Sintered Compact Sputtering Target
EP2503020A4 (en) * 2009-11-17 2013-07-24 Jx Nippon Mining & Metals Corp PROCESS FOR STORING A LANTHANOXIDE TARGET AND VACUUM PACKED LANTHANOXIDE TARGET
US8753491B2 (en) 2009-11-13 2014-06-17 Semiconductor Energy Laboratory Co., Ltd. Method for packaging target material and method for mounting target
EP2682497A4 (en) * 2011-03-01 2014-08-13 Jx Nippon Mining & Metals Corp METHOD FOR STORING A METAL LANTHANE TARGET, TARGET VACUUM SEALED METAL LANTHANE AND THIN FILM FORMED BY CATHODIC SPUTATION USING A METAL LANTHANE TARGET
US9013009B2 (en) 2011-01-21 2015-04-21 Jx Nippon Mining & Metals Corporation Method for producing high-purity lanthanum, high-purity lanthanum, sputtering target formed from high-purity lanthanum, and metal gate film having highy-purity lanthanum as main component
US9347130B2 (en) 2009-03-27 2016-05-24 Jx Nippon Mining & Metals Corporation Lanthanum target for sputtering
US9382612B2 (en) 2009-03-31 2016-07-05 Jx Nippon Mining & Metals Corporation Lanthanum target for sputtering

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CN102417042A (zh) * 2011-07-25 2012-04-18 武汉科技大学 易水化粉末标准样品/物质的包装与贮存方法
CN104309865A (zh) * 2014-05-30 2015-01-28 微密科技(无锡)有限公司 一种防颗粒污染的包装方法
JP6178455B1 (ja) * 2016-03-30 2017-08-09 Ｊｘ金属株式会社 円筒型スパッタリングターゲット及びその梱包方法
JP6348940B2 (ja) * 2016-09-21 2018-06-27 Ｊｘ金属株式会社 円筒型焼結体及びその梱包方法
JP6885981B2 (ja) * 2019-03-29 2021-06-16 Ｊｘ金属株式会社 スパッタリングターゲットの梱包物の作製方法及び輸送方法

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JP2000073054A (ja) * 1998-08-31 2000-03-07 Toyota Motor Corp 酸化防止剤およびその使用方法
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100272596A1 (en) * 2007-12-28 2010-10-28 Nippon Mining And Metals Co., Ltd. High-Purity Lanthanum, Sputtering Target Comprising High-Purity Lanthanum, and Metal Gate Film Mainly Comprising High-Purity Lanthanum
US8980169B2 (en) 2007-12-28 2015-03-17 Jx Nippon Mining & Metals Corporation High-purity lanthanum, sputtering target comprising high-purity lanthanum, and metal gate film mainly comprising high-purity lanthanum
US20110114481A1 (en) * 2008-07-07 2011-05-19 Jx Nippon Mining & Metals Corporation Lanthanum Oxide-based Sintered Compact, Sputtering Target Composed of said Sintered Compact, Method of Producing Lanthanum Oxide-based Sintered Compact, and Method of Producing Sputtering Target based on said Production Method
US20110114482A1 (en) * 2008-07-07 2011-05-19 Jx Nippon Mining & Metals Corporation Oxide Sintered Compact, Sputtering Target Composed of the Sintered Compact, and Method of Producing the Sintered Compact and the Sintered Compact Sputtering Target
US9347130B2 (en) 2009-03-27 2016-05-24 Jx Nippon Mining & Metals Corporation Lanthanum target for sputtering
US9382612B2 (en) 2009-03-31 2016-07-05 Jx Nippon Mining & Metals Corporation Lanthanum target for sputtering
US8753491B2 (en) 2009-11-13 2014-06-17 Semiconductor Energy Laboratory Co., Ltd. Method for packaging target material and method for mounting target
EP2503020A4 (en) * 2009-11-17 2013-07-24 Jx Nippon Mining & Metals Corp PROCESS FOR STORING A LANTHANOXIDE TARGET AND VACUUM PACKED LANTHANOXIDE TARGET
US8911600B2 (en) 2009-11-17 2014-12-16 Jx Nippon Mining & Metals Corporation Method of storing lanthanum oxide target, and vacuum-sealed lanthanum oxide target
US9013009B2 (en) 2011-01-21 2015-04-21 Jx Nippon Mining & Metals Corporation Method for producing high-purity lanthanum, high-purity lanthanum, sputtering target formed from high-purity lanthanum, and metal gate film having highy-purity lanthanum as main component
EP2682497A4 (en) * 2011-03-01 2014-08-13 Jx Nippon Mining & Metals Corp METHOD FOR STORING A METAL LANTHANE TARGET, TARGET VACUUM SEALED METAL LANTHANE AND THIN FILM FORMED BY CATHODIC SPUTATION USING A METAL LANTHANE TARGET
JP2014167167A (ja) * 2011-03-01 2014-09-11 Jx Nippon Mining & Metals Corp 金属ランタンターゲットの保管方法、真空密封した金属ランタンターゲット及び金属ランタンターゲットを用いてスパッタリングにより形成した薄膜

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WO2010050409A1 (ja) 2010-05-06
TW201016551A (en) 2010-05-01
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KR101290941B1 (ko) 2013-07-29
TWI472458B (zh) 2015-02-11

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