WO2022038795A1 - Cible de pulvérisation de métal précieux - Google Patents

Cible de pulvérisation de métal précieux Download PDF

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Publication number
WO2022038795A1
WO2022038795A1 PCT/JP2020/034659 JP2020034659W WO2022038795A1 WO 2022038795 A1 WO2022038795 A1 WO 2022038795A1 JP 2020034659 W JP2020034659 W JP 2020034659W WO 2022038795 A1 WO2022038795 A1 WO 2022038795A1
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WO
WIPO (PCT)
Prior art keywords
sputtering
sputtering target
carbon content
surface roughness
target
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Application number
PCT/JP2020/034659
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English (en)
Japanese (ja)
Inventor
英士 高田
孝博 小林
幸健 仲野
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松田産業株式会社
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Publication date
Application filed by 松田産業株式会社 filed Critical 松田産業株式会社
Priority claimed from JP2020153472A external-priority patent/JP7140164B2/ja
Publication of WO2022038795A1 publication Critical patent/WO2022038795A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • 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

Definitions

  • the present invention relates to a noble metal sputtering target that is most suitable for forming a thin film in the semiconductor field.
  • Sputtering is used to form thin films in fine wiring, MEMS, optical devices, LEDs, organic EL, high frequency devices, quartz, etc. in the semiconductor field.
  • an inert gas mainly argon gas
  • a target a plate-shaped film forming material, also called a sputtering target
  • the inert gas atom is ionized, and the gas ion is made to collide with the target surface at high speed and hit violently. This is a technique for forming a thin film by adhering and depositing on the surface.
  • Sputtering can form a film even on materials that are difficult to vacuum-deposit, such as refractory metals and alloys, and has the advantage of being able to handle a wide range of film-forming materials.
  • a sputtering target is subjected to preliminary sputtering for a certain period of time before use (called pre-sputtering) in order to stabilize its sputtering characteristics.
  • Pre-sputtering does not particularly contribute to film formation, but abnormal discharge during pre-sputtering may damage the sputtering target, and frequent generation of particles during pre-sputtering unnecessarily contaminates the inside of the sputtering chamber. There is a problem of doing.
  • An object of the present invention is to provide a precious metal sputtering target capable of suppressing the occurrence of abnormal discharge during pre-sputtering.
  • One aspect of the present invention capable of solving the above problems is a noble metal sputtering target characterized in that the surface roughness Ra of the surface to be sputtered is 10 ⁇ m or less and the carbon content is 10 wtppm or less.
  • the present invention has an excellent effect that the occurrence of abnormal discharge during pre-sputtering can be suppressed.
  • Au sputtering target It is a graph which shows the number of abnormal discharges at the time of pre-sputtering with respect to the surface roughness.
  • Au sputtering target It is a graph which shows the number of abnormal discharges at the time of pre-sputtering with respect to a carbon content.
  • Pt sputtering target It is a graph which shows the number of abnormal discharges at the time of pre-sputtering with respect to the surface roughness.
  • Pt sputtering target It is a graph which shows the number of abnormal discharges at the time of pre-sputtering with respect to a carbon content.
  • Pd sputtering target It is a graph which shows the number of abnormal discharges at the time of pre-sputtering with respect to the surface roughness.
  • Pd sputtering target is a graph showing the number of abnormal discharges during pre-sputtering with respect to the carbon content.
  • Ag sputtering target It is a graph which shows the number of abnormal discharges at the time of pre-sputtering with respect to the surface roughness.
  • Ag sputtering target is a graph showing the number of abnormal discharges during pre-sputtering with respect to the carbon content. It is a schematic diagram which shows the measurement point of the surface roughness of a sputtering target.
  • Sputtering is a technique in which argon ions collide with the surface of a sputtering target, the particles of the film-forming material constituting the sputtering target are violently ejected, and the particles are deposited on the surface of the substrate facing the target to form a thin film. It is called the surface where the surface of the sputtering target, which is opposed to the substrate and contributes to film formation, is sputtered by the collision of argon ions and the ejection of particles. It is known that the surface condition of the surface to be sputtered affects the sputtering characteristics (abnormal discharge, etc.), but the optimum surface condition greatly differs depending on the material of the sputtering target.
  • the optimum surface condition of a sputtering target made of a specific material is applied to the surface condition of a sputtering target made of another material, the same sputtering characteristics may not always be obtained.
  • the optimum surface condition for sputtering characteristics has not been known so far.
  • the noble metal sputtering target is an expensive material, shortening the pre-sputtering time is extremely effective from the viewpoint of cost, and it is important to find the optimum surface state for the noble metal sputtering target.
  • An embodiment of the present invention is a noble metal sputtering target, characterized in that the surface roughness Ra of the surface to be sputtered is 10 ⁇ m or less.
  • the surface roughness Ra of the surface to be sputtered is 10 ⁇ m or less.
  • the embodiment of the present invention is characterized in that the carbon content as an impurity is 10 wtppm or less.
  • the noble metal sputtering target tends to have carbon adhered to it during cleaning in the manufacturing process or from the atmosphere, which causes an abnormal discharge during pre-sputtering.
  • By setting the carbon content to 10 wtppm or less it is possible to suppress such abnormal discharge.
  • a preferred embodiment has a carbon content of 5 wtppm or less, and a more preferred embodiment has a carbon content of 2 wtppm or less.
  • a noble metal sputtering target means a sputtering target made of a single metal of gold, platinum, palladium, or silver, and means an alloy sputtering target that partially contains a noble metal such as a silver alloy. do not do.
  • a single metal unlike the case where the material of the sputtering target is an alloy, the optimum surface state for the sputtering characteristics changes, so that it is difficult to apply the optimum surface state as it is in the case of an alloy.
  • a single metal does not mean to exclude those containing a small amount of other metal components as impurities, and specifically, a total of 1000 wtppm or less of metal impurities may be contained. ..
  • Metal impurities can be analyzed using glow discharge mass spectrometry (GD-MS). If the content of each metal impurity is less than the lower limit of analysis, the lower limit of analysis is calculated as the content.
  • the noble metal sputtering target has different easiness of taking in impurities depending on the type of noble metal, it is particularly effective to limit the content of impurities according to the type of noble metal.
  • the carbon content is preferably 5 wtppm or less.
  • the carbon content is preferably 10 wtppm or less.
  • Au sputtering target An Au raw material having a purity of 4N was melted in a vacuum using a high-purity alumina crucible to prepare an Au ingot. The obtained Au ingot was forged, rolled, and heat-treated to be processed into a sputtering target shape. After that, the surface roughness of the surface to be sputtered was adjusted by lathe processing and CMP polishing of the sputtering target. In addition, in order to investigate the relationship between the carbon content and abnormal discharge, the standard sample is one that does not use lubricating oil when processing the ingot into a sputtering target shape and prevents carbon contamination. A certain amount of carbon powder was added to adjust the carbon content in the sputtering target.
  • Table 1 shows Au sputtering targets (samples) with adjusted surface roughness and carbon content.
  • pre-sputtering was performed under the following conditions, and the number of abnormal discharges was measured by the abnormal discharge monitor attached to the sputtering device.
  • the surface roughness was observed.
  • Ra exceeded 10 ⁇ m
  • the number of abnormal discharges increased sharply.
  • the number of abnormal discharges increased sharply after the carbon content exceeded 5 wtppm.
  • Sputtering device Magnetron system with built-in power supply Manufactured by Shinko Seiki (model: SDH10311) DC power supply: Kyosan Electric Manufacturing Co., Ltd. (Model: HPK06ZI) Power: 0.5kW-1.5kW Pressure: 0.2-0.4 Pa Wafer size: 6 inches Target size: 8 inches Pre-sputtering time: 20 minutes
  • Pt sputtering target A Pt raw material having a purity of 4N was melted in a vacuum using a high-purity alumina crucible to prepare a Pt ingot. The obtained Pt ingot was forged, rolled, and heat-treated to be processed into a sputtering target shape. After that, the surface roughness of the surface to be sputtered was adjusted by lathe processing and CMP polishing of the sputtering target. In addition, when processing the ingot into the target shape, no lubricating oil is used, and the standard sample is one that prevents carbon contamination, and a certain amount of carbon powder is added during dissolution in order to investigate the relationship between the carbon content and abnormal discharge. Addition was added to adjust the carbon content in the sputtering target.
  • Table 2 shows Pt sputtering targets (samples) with adjusted surface roughness and carbon content.
  • pre-sputtering was performed under the above pre-sputtering conditions, and the number of abnormal discharges was measured by the abnormal discharge monitor attached to the sputtering device.
  • the number of abnormal discharges increased sharply.
  • the number of abnormal discharges increased sharply after the carbon content exceeded 10 wtppm.
  • Pd sputtering target A Pd raw material having a purity of 3N5 was melted in vacuum using an alumina crucible to prepare an ingot of Pd. The obtained Pd ingot was forged, rolled, and heat-treated to be processed into a sputtering target shape. After that, the surface roughness of the surface to be sputtered was adjusted by lathe processing and CMP polishing of the sputtering target. In addition, when processing the Pd ingot into the target shape, the standard sample is one that does not use lubricating oil and prevents carbon contamination, and the carbon powder is kept constant during melting in order to investigate the relationship between the carbon content and abnormal discharge. The amount was added to adjust the carbon content in the sputtering target.
  • Table 3 shows Pd sputtering targets (samples) with adjusted surface roughness and carbon content.
  • pre-sputtering was performed under the above pre-sputtering conditions, and the number of abnormal discharges was measured by the abnormal discharge monitor attached to the sputtering device.
  • the number of abnormal discharges increased sharply.
  • the number of abnormal discharges increased sharply after the carbon content exceeded 10 wtppm.
  • An Ag raw material having a purity of 4N5 was melted in a vacuum using a high-purity carbon crucible to prepare an Ag ingot.
  • the obtained Ag ingot was forged, rolled, and heat-treated to be processed into a sputtering target shape. After that, the surface roughness of the surface to be sputtered was adjusted by lathe processing and CMP polishing of the sputtering target.
  • the standard sample is one that does not use lubricating oil and prevents carbon contamination, and the carbon powder is kept constant during melting in order to investigate the relationship between the carbon content and abnormal discharge. The amount was added to adjust the carbon content in the sputtering target.
  • Table 4 shows Ag sputtering targets (samples) with adjusted surface roughness and carbon content.
  • pre-sputtering was performed under the above pre-sputtering conditions, and the number of abnormal discharges was measured by the abnormal discharge monitor attached to the sputtering device. After the surface roughness Ra exceeded 5 ⁇ m, the number of abnormal discharges increased sharply. Further, as shown in FIG. 8, the number of abnormal discharges increased sharply after the carbon content exceeded 5 wtppm.
  • the noble metal sputtering target according to the embodiment of the present invention is useful for forming a thin film in a high frequency device, a crystal, a MEMS, an optical device, an LED, an organic EL, and the like.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Electrodes Of Semiconductors (AREA)

Abstract

Dans la présente invention, une cible de pulvérisation de métal précieux a une rugosité de surface Ra de pulvérisation inférieure ou égale à 10 µm et une teneur en carbone inférieure ou égale à 10 ppm en poids. Une cible de pulvérisation d'or a une rugosité de surface Ra de pulvérisation inférieure ou égale à 10 µm et une teneur en carbone inférieure ou égale à 5 ppm en poids. Une cible de pulvérisation de platine a une rugosité de surface Ra de pulvérisation inférieure ou égale à 5 µm et une teneur en carbone inférieure ou égale à 10 ppm en poids. Une cible de pulvérisation de palladium a une rugosité de surface Ra de pulvérisation inférieure ou égale à 5 µm et une teneur en carbone inférieure ou égale à 10 ppm en poids. Une cible de pulvérisation d'argent a une rugosité de surface Ra de pulvérisation inférieure ou égale à 10 µm et une teneur en carbone inférieure ou égale à 5 ppm en poids. La présente invention concerne une cible de pulvérisation de métal précieux hautement appropriée pour la formation de films minces dans le domaine des semi-conducteurs, et résout le problème de fourniture d'une cible de pulvérisation de métal précieux qui peut supprimer une décharge électrique anormale qui pourrait se produire pendant la pré-pulvérisation.
PCT/JP2020/034659 2020-08-17 2020-09-14 Cible de pulvérisation de métal précieux WO2022038795A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2020137355 2020-08-17
JP2020-137355 2020-08-17
JP2020153472A JP7140164B2 (ja) 2020-08-17 2020-09-14 貴金属スパッタリングターゲット
JP2020-153472 2020-09-14

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WO2022038795A1 true WO2022038795A1 (fr) 2022-02-24

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11269639A (ja) * 1998-03-24 1999-10-05 Sumitomo Metal Mining Co Ltd スパッタリングターゲットの再生方法
JP2001140063A (ja) * 1999-09-23 2001-05-22 Praxair St Technol Inc 延長された寿命を有するスパッタターゲット
JP2001316808A (ja) * 2000-05-09 2001-11-16 Toshiba Corp スパッタリングターゲット
JP2002146521A (ja) * 2000-11-10 2002-05-22 Nikko Materials Co Ltd 金ターゲットの製造方法
JP2006225696A (ja) * 2005-02-16 2006-08-31 Toshiba Corp スパッタリングターゲット、高屈折率膜とその製造方法、およびそれを用いた反射防止膜とディスプレイ装置
WO2010038642A1 (fr) * 2008-09-30 2010-04-08 日鉱金属株式会社 Cible de pulvérisation de cuivre de haute pureté ou d’alliage de cuivre de haute pureté, procédé pour la fabrication de la cible de pulvérisation, et film pulvérisé de cuivre de haute pureté ou d’alliage de cuivre de haute pureté
WO2019187311A1 (fr) * 2018-03-26 2019-10-03 Ｊｘ金属株式会社 Élément cible de pulvérisation et son procédé de production

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5159962B1 (ja) * 2012-01-10 2013-03-13 三菱マテリアル株式会社 導電性膜形成用銀合金スパッタリングターゲットおよびその製造方法
JP6729344B2 (ja) * 2016-12-20 2020-07-22 三菱マテリアル株式会社 Ａｇ合金スパッタリングターゲットおよびＡｇ合金膜

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11269639A (ja) * 1998-03-24 1999-10-05 Sumitomo Metal Mining Co Ltd スパッタリングターゲットの再生方法
JP2001140063A (ja) * 1999-09-23 2001-05-22 Praxair St Technol Inc 延長された寿命を有するスパッタターゲット
JP2001316808A (ja) * 2000-05-09 2001-11-16 Toshiba Corp スパッタリングターゲット
JP2002146521A (ja) * 2000-11-10 2002-05-22 Nikko Materials Co Ltd 金ターゲットの製造方法
JP2006225696A (ja) * 2005-02-16 2006-08-31 Toshiba Corp スパッタリングターゲット、高屈折率膜とその製造方法、およびそれを用いた反射防止膜とディスプレイ装置
WO2010038642A1 (fr) * 2008-09-30 2010-04-08 日鉱金属株式会社 Cible de pulvérisation de cuivre de haute pureté ou d’alliage de cuivre de haute pureté, procédé pour la fabrication de la cible de pulvérisation, et film pulvérisé de cuivre de haute pureté ou d’alliage de cuivre de haute pureté
WO2019187311A1 (fr) * 2018-03-26 2019-10-03 Ｊｘ金属株式会社 Élément cible de pulvérisation et son procédé de production

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TW202210646A (zh) 2022-03-16
TWI830035B (zh) 2024-01-21

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