JP2020514230A - 窒化ホウ素ナノチューブの精製方法 - Google Patents
窒化ホウ素ナノチューブの精製方法 Download PDFInfo
- Publication number
- JP2020514230A JP2020514230A JP2019548538A JP2019548538A JP2020514230A JP 2020514230 A JP2020514230 A JP 2020514230A JP 2019548538 A JP2019548538 A JP 2019548538A JP 2019548538 A JP2019548538 A JP 2019548538A JP 2020514230 A JP2020514230 A JP 2020514230A
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- period
- bnnt material
- bnnt
- boron nitride
- 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.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/14—Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium
- C01B35/146—Compounds containing boron and nitrogen, e.g. borazoles
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
Description
Claims (21)
- 窒化ホウ素ナノチューブ(BNNT)から不純物を取り除くための精製方法であって、前記精製方法は、
前記BNNT材料を第1温度で第1期間加熱し、ホウ素不純物を取り除く工程と、
前記BNNT材料を、前記第1温度よりも高い第2温度で第2期間加熱し、窒化ホウ素不純物を取り除く工程と、
前記BNNT材料を、前記第2温度よりも低い第3温度で第3期間加熱して、酸化ホウ素不純物を取り除く工程と、
を含む、ことを特徴とする窒化ホウ素ナノチューブ精製方法。 - 前記第1温度は約500〜650℃であることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記第1期間は約0.16〜12時間であることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 不活性ガス及び水素供給原料の存在下において、前記BNNT材料を第1温度で第1期間加熱することを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記第2温度は約650〜800℃であることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記第2期間は約1〜12時間であることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記第3の温度は約500〜650℃であることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記第3期間は約0.16〜1時間であることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記第1期間、前記第2期間、及び前記第3期間はおよそ、時間量が同じであることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記BNNT材料をベーク期間の間、ベーク温度にてプリベークし、炭素不純物を取り除くことを更に含むことを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- 前記ベーク温度は約400〜500℃であり、前記ベーク期間は約0.5〜3時間であることを特徴とする、請求項10に記載の窒化ホウ素ナノチューブ精製方法。
- 前記プリベークは、前記BNNT材料を第1温度で第1期間加熱する前に生じることを特徴とする、請求項10に記載の窒化ホウ素ナノチューブ精製方法。
- 前記BNNT材料は、オゾンを含む雰囲気でプリベークされることを特徴とする、請求項10に記載の窒化ホウ素ナノチューブ精製方法。
- 前記不活性ガスは窒素であることを特徴とする、請求項4に記載の窒化ホウ素ナノチューブ精製方法。
- 前記水素供給原料は、水蒸気及び水素ガスのうち少なくとも1つであることを特徴とする、請求項4に記載の窒化ホウ素ナノチューブ精製方法。
- 前記水素供給原料は水蒸気を含み、前記窒素ガス中の水蒸気の量は、乾燥窒素ガスを使用し、前記乾燥窒素ガスを、約30〜100℃の温度の飽和水蒸気条件に通すことにより制御されることを特徴とする、請求項15に記載の窒化ホウ素ナノチューブ精製方法。
- 前記BNNT材料は、0.1〜12気圧の圧力を有する雰囲気で加熱されることを特徴とする、請求項1に記載の窒化ホウ素ナノチューブ精製方法。
- BNNT材料の精製方法であって、前記精製方法は、
酸素リッチな環境で、前記BNNT材料を500〜650℃の第1温度で、0.16〜12時間の第1期間加熱し、ホウ素不純物を取り除くことと、
前記BNNT材料を、650〜800℃の第2温度で、1〜12時間の第2期間加熱し、窒化ホウ素不純物を取り除くことと、
前記BNNT材料を、500〜650℃の第3温度で、0.16〜1時間の第3期間加熱し、酸化ホウ素不純物を取り除くことと、
を含むことを特徴とする、窒化ホウ素ナノチューブ精製方法。 - 前記BNNT材料を、400〜500℃のベーク温度で、約0.5〜3時間のベーク期間加熱し、炭素不純物を取り除くことを更に含むことを特徴とする、請求項18に記載の窒化ホウ素ナノチューブ精製方法。
- 前記BNNT材料は、オゾンを含む環境でプリベークされることを特徴とする、請求項19に記載の窒化ホウ素ナノチューブ精製方法。
- 前記BNNT材料は、0.1〜12気圧の圧力を有する雰囲気で加熱されることを特徴とする、請求項18に記載の窒化ホウ素ナノチューブ精製方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201662427506P | 2016-11-29 | 2016-11-29 | |
US62/427,506 | 2016-11-29 | ||
PCT/US2017/063729 WO2018102423A1 (en) | 2016-11-29 | 2017-11-29 | Boron nitride nanotube purification |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2020514230A true JP2020514230A (ja) | 2020-05-21 |
JP7029465B2 JP7029465B2 (ja) | 2022-03-03 |
Family
ID=62242636
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2019548538A Active JP7029465B2 (ja) | 2016-11-29 | 2017-11-29 | 窒化ホウ素ナノチューブの精製方法 |
Country Status (7)
Country | Link |
---|---|
US (2) | US11629054B2 (ja) |
EP (1) | EP3548434B1 (ja) |
JP (1) | JP7029465B2 (ja) |
KR (2) | KR20230058179A (ja) |
AU (1) | AU2017367089B2 (ja) |
CA (1) | CA3043507A1 (ja) |
WO (1) | WO2018102423A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022102741A1 (ja) * | 2020-11-16 | 2022-05-19 | 日立金属株式会社 | 窒化ホウ素ナノチューブの製造方法 |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3617137B1 (en) | 2017-02-07 | 2023-08-09 | Bnnt, Llc | Boron nitride nanotube vibration damping |
EP3755656A4 (en) * | 2018-02-19 | 2021-11-24 | Bnnt, Llc | BNNT THERMAL MANAGEMENT MATERIALS FOR HIGH POWER SYSTEMS |
WO2020010458A1 (en) * | 2018-07-11 | 2020-01-16 | National Research Council Of Canada | Process and apparatus for purifying bnnt |
JP6942894B2 (ja) * | 2018-10-29 | 2021-09-29 | 日立金属株式会社 | 窒化ホウ素ナノ物質の製造方法および窒化ホウ素ナノ物質、複合材料の製造方法および複合材料、ならびに窒化ホウ素ナノ物質の精製方法 |
DE112020000350T5 (de) * | 2019-01-07 | 2021-09-23 | Bnnt, Llc | Optimierung einer Bornitrid-Nanoröhren-Vibrationsdämpfung |
US11254571B1 (en) * | 2019-01-11 | 2022-02-22 | United States Of America As Represented By The Secretary Of The Air Force | Purification and enrichment of boron nitride nanotube feedstocks |
US20200231439A1 (en) * | 2019-01-17 | 2020-07-23 | College Of William & Mary | Methods and compositions for highly purified boron nitride nanotubes |
KR102393063B1 (ko) * | 2019-10-21 | 2022-05-03 | 한국과학기술연구원 | 질화붕소 나노튜브의 정제방법 |
KR102367735B1 (ko) * | 2019-12-20 | 2022-02-25 | 한국전자기술연구원 | 전단응력을 이용한 질화붕소나노튜브의 물리적 정제방법 |
CN112520714A (zh) * | 2020-03-20 | 2021-03-19 | 山东晶亿新材料有限公司 | 一种六方氮化硼及其制备方法和应用 |
KR102534772B1 (ko) | 2021-02-17 | 2023-05-22 | 한국과학기술연구원 | 자기정렬된 질화붕소나노튜브-탄소나노튜브 혼합체를 이용한 전계효과트랜지스터 및 그 제조방법 |
KR102601243B1 (ko) | 2021-03-15 | 2023-11-13 | 한국과학기술연구원 | 질화붕소나노튜브 정제방법 및 질화붕소나노튜브 정제 조성물 |
KR102568024B1 (ko) * | 2021-03-30 | 2023-08-22 | 한국과학기술연구원 | Bnnt 정제장치 및 방법 |
WO2023096720A2 (en) * | 2021-10-29 | 2023-06-01 | Bnnt, Llc | Boron nitride nanotube intermediaries for nanomaterials |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS516198A (ja) * | 1974-07-08 | 1976-01-19 | Hitachi Ltd | Ritsuhoshochitsukahosono seiseihoho |
JP2003505332A (ja) * | 1999-07-21 | 2003-02-12 | ハイピリオン カタリシス インターナショナル インコーポレイテッド | 多層カーボンナノチューブの酸化方法 |
US20080069758A1 (en) * | 2006-05-09 | 2008-03-20 | Ada Technologies, Inc. | Carbon Nanotube Purification and Separation System |
US20100074832A1 (en) * | 2004-03-17 | 2010-03-25 | California Institute Of Technology | Methods for purifying carbon materials |
US8734748B1 (en) * | 2010-09-28 | 2014-05-27 | The United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration | Purifying nanomaterials |
JP2016521240A (ja) * | 2013-04-18 | 2016-07-21 | ナショナル リサーチ カウンシル オブ カナダ | 窒化ホウ素ナノチューブ及びその製造方法 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6967011B1 (en) | 2002-12-02 | 2005-11-22 | The United States Of America As Represented By The United States Department Of Energy | Method for synthesizing extremely high-temperature melting materials |
JP5059589B2 (ja) * | 2007-12-27 | 2012-10-24 | 帝人株式会社 | 窒化ホウ素ナノ繊維及びその製造方法 |
US20100192535A1 (en) | 2009-02-04 | 2010-08-05 | Smith Michael W | Boron nitride nanotube fibrils and yarns |
DE112013007154B4 (de) | 2013-06-14 | 2018-10-31 | Yeditepe Universitesi | Herstellungsverfahren für Bornitrid-Nanoröhren |
-
2017
- 2017-11-29 JP JP2019548538A patent/JP7029465B2/ja active Active
- 2017-11-29 CA CA3043507A patent/CA3043507A1/en active Pending
- 2017-11-29 AU AU2017367089A patent/AU2017367089B2/en active Active
- 2017-11-29 EP EP17876878.4A patent/EP3548434B1/en active Active
- 2017-11-29 US US16/349,483 patent/US11629054B2/en active Active
- 2017-11-29 KR KR1020237013154A patent/KR20230058179A/ko not_active Application Discontinuation
- 2017-11-29 WO PCT/US2017/063729 patent/WO2018102423A1/en active Search and Examination
- 2017-11-29 KR KR1020197017444A patent/KR102524467B1/ko active IP Right Grant
-
2023
- 2023-03-14 US US18/121,086 patent/US20230286801A1/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS516198A (ja) * | 1974-07-08 | 1976-01-19 | Hitachi Ltd | Ritsuhoshochitsukahosono seiseihoho |
JP2003505332A (ja) * | 1999-07-21 | 2003-02-12 | ハイピリオン カタリシス インターナショナル インコーポレイテッド | 多層カーボンナノチューブの酸化方法 |
US20100074832A1 (en) * | 2004-03-17 | 2010-03-25 | California Institute Of Technology | Methods for purifying carbon materials |
US20080069758A1 (en) * | 2006-05-09 | 2008-03-20 | Ada Technologies, Inc. | Carbon Nanotube Purification and Separation System |
US8734748B1 (en) * | 2010-09-28 | 2014-05-27 | The United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration | Purifying nanomaterials |
JP2016521240A (ja) * | 2013-04-18 | 2016-07-21 | ナショナル リサーチ カウンシル オブ カナダ | 窒化ホウ素ナノチューブ及びその製造方法 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022102741A1 (ja) * | 2020-11-16 | 2022-05-19 | 日立金属株式会社 | 窒化ホウ素ナノチューブの製造方法 |
JPWO2022102741A1 (ja) * | 2020-11-16 | 2022-05-19 | ||
JP7276625B2 (ja) | 2020-11-16 | 2023-05-18 | 株式会社プロテリアル | 窒化ホウ素ナノチューブの製造方法 |
Also Published As
Publication number | Publication date |
---|---|
US20230286801A1 (en) | 2023-09-14 |
JP7029465B2 (ja) | 2022-03-03 |
KR20230058179A (ko) | 2023-05-02 |
EP3548434A1 (en) | 2019-10-09 |
US20190292052A1 (en) | 2019-09-26 |
KR102524467B1 (ko) | 2023-04-24 |
KR20190087492A (ko) | 2019-07-24 |
WO2018102423A1 (en) | 2018-06-07 |
EP3548434B1 (en) | 2023-03-15 |
AU2017367089B2 (en) | 2021-09-30 |
EP3548434A4 (en) | 2020-06-24 |
US11629054B2 (en) | 2023-04-18 |
AU2017367089A1 (en) | 2019-06-06 |
CA3043507A1 (en) | 2018-06-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP2020514230A (ja) | 窒化ホウ素ナノチューブの精製方法 | |
EP2094622B1 (de) | Verfahren zur herstellung eines gegenstandes zumindest teilweise mit siliziumkarbidgefüge aus einem rohling aus einem kohlenstoffhaltigen material | |
JP2009269797A (ja) | 炭化ケイ素粉末の製造方法 | |
JP2008050201A (ja) | 炭化ケイ素粉末の製造方法及び炭化ケイ素粉末 | |
CN102810359B (zh) | 化学气相沉积法制备同轴碳化硅/二氧化硅纳米电缆的方法 | |
KR101005115B1 (ko) | 표면에 그라파이트 나노 구조층을 갖는 셀룰로오스 탄화물 구조체의 합성방법 | |
KR101549477B1 (ko) | 고순도 탄화규소 분말의 제조방법 | |
JP2007084369A (ja) | TiC超微粒子又はTiO2超微粒子担持カーボンナノチューブ、及びTiCナノチューブとこれらの製造方法 | |
JP5261230B2 (ja) | ケイ素微粒子発光体の製造方法 | |
JP2009298610A (ja) | 炭化ケイ素チューブの製造方法 | |
JP6454214B2 (ja) | シリカ及びその製造方法 | |
US9399583B2 (en) | Silicon carbide powder production method | |
JPH02184511A (ja) | 多孔質グラファイトの製造方法 | |
JP2009269798A (ja) | 炭化ケイ素粒子およびその製造方法 | |
US9908782B2 (en) | Method for synthesis of boron suboxide | |
KR20120012345A (ko) | 탄화 규소 및 이의 제조 방법 | |
US9409782B2 (en) | Method of fabricating silicon carbide powder | |
JP2016079057A (ja) | キラルな固体金属及び固体複合体、並びにそれらの製造方法 | |
KR102190734B1 (ko) | 균일한 나노 사이즈의 기공을 갖는 그래핀의 제조방법 | |
DE102021131748B3 (de) | Verfahren zum Herstellen von hochreinem Siliziumkarbid-Pulver | |
US20210009422A1 (en) | Carbon purification method and carbon product | |
KR102622058B1 (ko) | 고순도 쿼츠 분말의 제조방법 | |
KR101978938B1 (ko) | 실리콘 카바이드 제조방법 및 이를 이용하여 제조된 실리콘 카바이드 | |
Yao et al. | CVD synthesis and purification of multi-walled carbon nanotubes | |
WO2023073145A1 (de) | Siliziumkarbidhaltiges material, präkursor-zusammensetzung und deren herstellungsverfahren |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A529 | Written submission of copy of amendment under article 34 pct |
Free format text: JAPANESE INTERMEDIATE CODE: A529 Effective date: 20190624 |
|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20201119 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20210826 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20210907 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20211207 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20220208 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20220218 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 7029465 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |