WO2004016824A1 - 導電性酸化物焼結体、同焼結体からなるスパッタリングターゲット及びこれらの製造方法 - Google Patents

導電性酸化物焼結体、同焼結体からなるスパッタリングターゲット及びこれらの製造方法 Download PDF

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WO2004016824A1
WO2004016824A1 PCT/JP2003/007483 JP0307483W WO2004016824A1 WO 2004016824 A1 WO2004016824 A1 WO 2004016824A1 JP 0307483 W JP0307483 W JP 0307483W WO 2004016824 A1 WO2004016824 A1 WO 2004016824A1
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sintered body
conductive oxide
oxide sintered
sputtering target
sintered compact
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French (fr)
Japanese (ja)
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Ryo Suzuki
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Nippon Mining Holdings Inc
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Nikko Materials Co Ltd
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Priority to US10/522,263 priority Critical patent/US7252794B2/en
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    • 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
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • 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
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    • 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D84/00—Integrated devices formed in or on semiconductor substrates that comprise only semiconducting layers, e.g. on Si wafers or on GaAs-on-Si wafers
    • H10D84/80—Integrated devices formed in or on semiconductor substrates that comprise only semiconducting layers, e.g. on Si wafers or on GaAs-on-Si wafers characterised by the integration of at least one component covered by groups H10D12/00 or H10D30/00, e.g. integration of IGFETs
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Definitions

  • the present invention relates to a conductive oxide sintered body suitable for an electrode of a dielectric thin film memory such as a DRAM and a FRAM, a bright sputtering target made of the sintered body, and a method of manufacturing the same.
  • the PTZ P b Z r X T i ⁇ 0 3
  • B ST BaS rT i 3
  • the above-mentioned conductive oxides have a problem that the sinterability is poor and the sintering density is extremely low.
  • the sputtering target obtained from such a low-density sintered body since the pores in the target have open pores, cutting powder and the like remain during the processing of the target, and the electrode There is a problem that the generation of particles is remarkably increased at the time of sputtering when forming the thin film.
  • targets with low sintering density are liable to cracks and chips during the manufacturing process, operation, and sputtering, which lowers the yield and makes it impossible to increase the sputtering power during sputtering.
  • a sintering aid to increase the sintering density.
  • JP 2000- 247739 in the literature that have been attempted to increase until the B i 2 0 3 to 0. OO lmo l ⁇ 0. 5mo 1 added 85% to 90% of relative density.
  • the present invention in order to solve the above problems, the addition amount and sintering conditions of B i 2 ⁇ 3 by improved, an improvement in the relative density of the S RRu_ ⁇ 3 based conductive oxide sintered body
  • a conductive oxide sintered body that suppresses the generation of particles during sputtering when forming a thin film and improves quality and yield, a sputtering target obtained from the sintered body, and a method for producing these. Task to do.
  • the present invention is a.
  • a sputtering target comprising the conductive oxide sintered body according to the above item 6, wherein the specific resistance is 500 ⁇ ⁇ cm or less.
  • Figure 1 is a diagram showing the relationship between B i 2 ⁇ 3 amount and resistivity and relative density when fired at 1700 ° C.
  • the present invention as the material of the sputtering target, relates DRAM, Berobusukai preparative S r Ru0 3 based conductive oxide can be used to form such dielectric thin film memory one thin film electrode of the FRAM, etc.
  • S RRu_ ⁇ 3 based conductive oxides results of density increase was evolving as goal of it is possible that the relative density to obtain a S r Ru_ ⁇ 3 based conductive oxide sintered body and the sputtering target is 93% or more It became.
  • the present invention further provides these production methods.
  • the SrRu 3 based conductive oxide sintered body and the sputtering target of the present invention can obtain a material having a specific resistance of 500 ⁇ cm or less and further a specific resistance of 300 ⁇ ⁇ cm or less, and are suitable as an electrode material. High conductivity can be obtained. As the relative density increases, the resistivity tends to further decrease.
  • the B i 2 0 3 as a sintering aid 0. 3mo l ⁇ l. 2mo 1 added. Preferably 0. The B i 2 ⁇ 3 5 (super) mo l ⁇ l. 0 mo 1 sintered added. Yotsute thereto, S RRu_ ⁇ the 3 based conductive oxide sintered body and the sputtering target, B i 2 ⁇ 3 0. 3m o 1 ⁇ :. L 2 mo 1, preferably B i 2 O 3 0 . 5 (super) mo 1 to 1.0 mo 1 is contained.
  • the thickness exceeds 1.2 mol, a second layer is formed in the sputtered film, which generates a Bi compound at the interface with the BSTO film or the PZT film, and causes a problem of deteriorating the dielectric characteristics.
  • the upper limit of the addition amount was set to 1.2 mol, more preferably 1 Omo 1.
  • Sintering temperature exceeds 1700 ° C when Ru0 2 evaporation becomes vigorous, generated by S r 2 Ru_ ⁇ 4, since conductivity decreases, it is necessary to not more than 1700 ° C.
  • the relative density obtained by the above is 93% or more density S RRu_ ⁇ 3 Keishirubeden oxide sintered evening one target is pores form in ⁇ Taichi rodents Bok is in the closed pores (open Since no pores remain), there is no residual cutting powder or the like at the time of target processing, and the generation of particles can be significantly reduced when a thin film for an electrode is formed by sputtering.
  • the high-density target has the effect of reducing the specific resistance as described above, and has the remarkable advantage that it can improve the product yield without cracking or chipping during the manufacturing process, operation, and even during sputtering. There is. Further, there is an effect that the sputter power can be increased at the time of sputtering and the production cost can be improved. Examples and comparative examples
  • the S r CO 3 powder and Ru0 2 powder having a purity of 4 N (99. 99%) of purity 5N (99. 999%) was used as a starting material, and both the powder in a molar ratio of 1: After weighing to be 1, pure water was mixed with a pole mill as a medium. The resulting slurry was dried in air, subjected to hot synthesis under conditions of 10 00 ° CX 10 hours to prepare a S r R u 0 3 single phase powder. Next, the B i 2 0 3 powder having a purity of 4N to S r Ru0 3 powder, 0 (no addition), 0.2, 0.5, 0.8, 1.0 and 1. added 2 mol% Each sample was then mixed and ground again with a pole mill.
  • Specific resistance judgment XXX ⁇ XX Specific resistance judgment: Specific resistance of 300 ⁇ ⁇ cm or less is indicated by ⁇ , and above is indicated by X.
  • FIG. 1 also shows the relationship between the added amount of Bi 2 O 3 and the specific resistance when firing at 1700 ° C. As shown in FIG. 1, 8 ⁇ 2 0 3 amount 0. 2 mo 1% or more, specific resistance can be achieved following 300 Omega cm.
  • Sputtering was performed using the target thus fabricated, and the particles on the 6-inch wafer were measured. As a result, there were 89, 14, and 13 particles with a size of 0.3 or more, respectively.
  • the relative density of any of the targets falling within the scope of the present invention was 93% or more, and the number of particles was 20 or less. Under the optimum sintering conditions at 1400 ° C to 1700 ° C, the relative density was improved.
  • Density S r R U_ ⁇ 3 based conductive oxide sintered body target relative density of the present invention is 9 3% or more, pores form in the target is in the closed pores (open pores remaining exist Therefore, no cutting powder or the like during target processing remains, and the generation of particles can be significantly reduced when a thin film for an electrode is formed by sputtering.
  • high-density targets have the effect of further reducing the specific resistance, and can improve product yield without cracking or chipping during the manufacturing process, operation, and even during sputtering.
  • sputtering power can be increased at the time of sputtering and the production cost can be increased.

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PCT/JP2003/007483 2002-08-06 2003-06-12 導電性酸化物焼結体、同焼結体からなるスパッタリングターゲット及びこれらの製造方法 Ceased WO2004016824A1 (ja)

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US10/522,263 US7252794B2 (en) 2002-08-06 2003-06-12 Electroconductive oxide sintered compact, sputtering target comprising the sintered compact and methods for producing them

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JP2002228165A JP4544501B2 (ja) 2002-08-06 2002-08-06 導電性酸化物焼結体、同焼結体からなるスパッタリングターゲット及びこれらの製造方法
JP2002-228165 2002-08-06

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JP (1) JP4544501B2 (enExample)
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JP4351213B2 (ja) * 2003-09-03 2009-10-28 日鉱金属株式会社 スパッタリング用ターゲット及びその製造方法
KR100881851B1 (ko) * 2004-03-01 2009-02-06 닛코킨조쿠 가부시키가이샤 고순도 루테니움 분말, 이 고순도 루테니움 분말을소결하여 얻는 스퍼터링 타겟트 및 이 타겟트를 스퍼터링하여 얻은 박막 및 고순도 루테니움 분말의 제조방법
US7686985B2 (en) * 2005-06-28 2010-03-30 Nippon Mining & Metals Co., Ltd Gallium oxide-zinc oxide sputtering target, method of forming transparent conductive film, and transparent conductive film
KR101004981B1 (ko) * 2005-06-28 2011-01-04 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 산화갈륨-산화아연계 스퍼터링 타겟, 투명 도전막의 형성방법 및 투명 도전막
US8118984B2 (en) * 2006-02-22 2012-02-21 Jx Nippon Mining & Metals Corporation Sintered sputtering target made of refractory metals
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KR100642929B1 (ko) 2006-11-10
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