JP4426525B2 - 多孔質材料及びその製造方法、並びにハニカム構造体 - Google Patents
多孔質材料及びその製造方法、並びにハニカム構造体 Download PDFInfo
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- JP4426525B2 JP4426525B2 JP2005503755A JP2005503755A JP4426525B2 JP 4426525 B2 JP4426525 B2 JP 4426525B2 JP 2005503755 A JP2005503755 A JP 2005503755A JP 2005503755 A JP2005503755 A JP 2005503755A JP 4426525 B2 JP4426525 B2 JP 4426525B2
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- silicon
- porous material
- silicon carbide
- silicon nitride
- nitrogen atmosphere
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- 239000011148 porous material Substances 0.000 title claims description 145
- 238000004519 manufacturing process Methods 0.000 title claims description 34
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 84
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 81
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 81
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 44
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 claims description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000010304 firing Methods 0.000 claims description 40
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 40
- 239000010703 silicon Substances 0.000 claims description 39
- 229910052710 silicon Inorganic materials 0.000 claims description 39
- 239000007789 gas Substances 0.000 claims description 38
- 238000005121 nitriding Methods 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 239000012298 atmosphere Substances 0.000 claims description 17
- 230000035699 permeability Effects 0.000 claims description 17
- 239000011230 binding agent Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
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- 238000012360 testing method Methods 0.000 description 19
- 238000005259 measurement Methods 0.000 description 18
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- 239000002994 raw material Substances 0.000 description 10
- 239000012300 argon atmosphere Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
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- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 4
- 238000005192 partition Methods 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052747 lanthanoid Inorganic materials 0.000 description 3
- 150000002602 lanthanoids Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
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- 150000002222 fluorine compounds Chemical class 0.000 description 2
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- 238000004898 kneading Methods 0.000 description 2
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- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
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- 239000012466 permeate Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
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- 230000001788 irregular Effects 0.000 description 1
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- 239000000155 melt Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 239000012071 phase Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
平均粒径が47μmの炭化珪素(SiC)80質量%、平均粒径が5μmの金属珪素(Si)粉末20質量%の合計に対し外比として、助剤としての化合物(以下、「助剤」ということがある)である炭酸ストロンチウム1質量%、造孔材である澱粉10質量%、バインダーであるメチルセルロース8質量%、界面活性剤1質量%、そして水を19質量%それぞれ添加、混合して焼成前の原料を作製し、それを混練機にて混練し、押出成形によりハニカム構造の成形体を作製した(上記、各比率(質量%)はSiC+Siを100とした場合の、それに対する質量%を意味する)。得られたハニカム構造の成形体を大気中で500℃に保持し、バインダーを除去した。その後、1.3Pa、アルゴン雰囲気中、1450℃で2時間焼成して(成形体の窒化前焼成)、ハニカム構造の珪素−炭化珪素多孔体を得た。珪素−炭化珪素多孔体を作製した後に、室温まで降温(冷却)し、室温で窒素雰囲気に切り換えた。そして、改めて1450℃まで昇温し、得られたハニカム構造の珪素−炭化珪素多孔体を、常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、窒化処理を施した後に、1750℃で4時間保持し(窒化時焼成条件)焼結体(ハニカムセラミックス構造体)を得た(作製条件を表1に示す)。ここで、表1において、「窒化前及び窒化の同一回焼成区分」とは、上記、珪素−炭化珪素多孔体を作製した後に、室温まで降温した後に窒化する(別焼成)か、降温せずに窒化する(同一焼成)かを区別することをいう。つまり、同一(回)焼成とは、珪素−炭化珪素多孔体を作製するときの焼成と、得られた珪素−炭化珪素多孔体を窒化するときの焼成とを、間に降温(冷却)工程を介さずに連続的に行うことをいい、別焼成とは、上記降温(冷却)工程を介して2回に分けて焼成することをいう。また、表1において、「(雰囲気切換え温度)」とは、上記珪素−炭化珪素多孔体を作製した後、窒化するときに、雰囲気を窒素雰囲気に切換えるが、そのときの温度をいう。得られた焼結体から4×3×40mm及びφ10×3mm等の試験片を切出し、下記の評価項目の測定を行った。測定結果を表3に示す。
開気孔率:水中重量法で測定した。
実施例1において、「ハニカム構造の珪素−炭化珪素多孔体を得た」後に、降温することなく、温度を1400℃に維持した状態で窒素雰囲気に切り換えた。その後、常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、窒化処理を施した後に、1750℃で4時間保持し(窒化時焼成条件)焼結体(ハニカムセラミックス構造体)を得た(作製条件を表1に示す)。その他の条件は、実施例1と同様にした。また、実施例1と同様にして、得られた焼結体から試験片を切出し、上記の評価項目の測定を行った。測定結果を表3に示す。
造孔材(実施例1においては、澱粉)を添加しなかった点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
助剤(実施例1においては、炭酸ストロンチウム)を添加しなかった点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
実施例1において、「1.3Pa、アルゴン雰囲気中、1450℃で2時間焼成して、ハニカム構造の珪素−炭化珪素多孔体を得た」ところを、「常圧(大気圧)、アルゴン雰囲気(酸素分圧10Pa)中、1450℃で2時間焼成して、ハニカム構造の珪素−炭化珪素多孔体を得た」とした点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
炭化珪素(SiC)の平均粒径を24μmとした点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
造孔材である澱粉の添加量を30質量%とした点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
造孔材の添加量を40質量%とした点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
実施例1において、炭化珪素と珪素との質量比を70:30とし、炭化珪素と珪素との質量の合計の、上記焼成前の原料全体の質量に対する比率は実施例1と同一にし、助剤と珪素との添加量の比が、実施例1における助剤と珪素の添加量の比と同一になるように助剤を添加し、さらに造孔材を添加しない点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして、上記の評価項目の測定を行った。測定結果を表3に示す。
炭化珪素(SiC)の平均粒径を68μmとした点以外は、実施例1と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
炭化珪素(SiC)の平均粒径を12μmとした点以外は、実施例7と同様にして焼結体を作製し(作製条件を表1に示す)、試験片を切出した。実施例1と同様にして上記の評価項目の測定を行った。測定結果を表3に示す。
助剤(実施例1においては、炭酸ストロンチウム)の添加量を3質量%とし、実施例1において、「ハニカム構造の珪素−炭化珪素多孔体を、常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、更に1750℃で4時間保持」した「窒化時焼成条件」を、「ハニカム構造の珪素−炭化珪素多孔体を、常圧(大気圧)、窒素雰囲気で1200℃で12時間保持」することとした。その他の条件は、実施例1と同様にした(作製条件を表1に示す)。また、実施例1と同様にして、得られた焼結体から試験片を切出し、上記の評価項目の測定を行った。測定結果を表3に示す。
実施例1において、「1.3Pa、アルゴン雰囲気中」を「常圧(大気圧)、アルゴン雰囲気(酸素分圧10Pa)中」とし、「常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、窒化処理を施した後に、1750℃で4時間保持し(窒化時焼成条件)焼結体(ハニカムセラミックス構造体)を得た」を「常圧(大気圧)、水素を5体積%混合した窒素雰囲気で1450℃で4時間保持し焼結体(ハニカムセラミックス構造体)を得た」とする。その他の条件は、実施例1と同様にした(作製条件を表1に示す)。また、実施例1と同様にして、得られた焼結体から試験片を切出し、上記の評価項目の測定を行った。測定結果を表3に示す。
実施例1において、「1.3Pa、アルゴン雰囲気中」を「常圧(大気圧)、アルゴン雰囲気(酸素分圧10Pa)中」とし、「珪素−炭化珪素多孔体を作製した後に、室温まで降温(冷却)し、室温で窒素雰囲気に切り換えた。そして、改めて1450℃まで昇温し、得られたハニカム構造の珪素−炭化珪素多孔体を、常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、窒化処理を施した後に、1750℃で4時間保持し(窒化時焼成条件)焼結体(ハニカムセラミックス構造体)を得た」を「珪素−炭化珪素多孔体を作製した後に、室温まで降温することなく、温度を1450℃に維持した状態で水素を5体積%混合した窒素雰囲気に切り換え、1450℃で4時間保持し焼結体(ハニカムセラミックス構造体)を得た」とする。その他の条件は、実施例1と同様にした(作製条件を表1に示す)。また、実施例1と同様にして、得られた焼結体から試験片を切出し、上記の評価項目の測定を行った。測定結果を表3に示す。
実施例1において、ハニカム構造の成形体を押出成形により作製し、大気中で500℃に保持してバインダーを除去した後に、常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、窒化処理を施した後に、1750℃で4時間保持した。得られた、窒化処理を施したハニカム構造の成形体は、焼結されておらず、触れると崩壊するため、試験片を切出すことができなかった(作製条件を表2に示す)。そのため、上記評価項目の測定はできなかった。
実施例1の「成形体の窒化前焼成」において、常圧(大気圧)、アルゴン雰囲気(酸素分圧100Pa)中、1450℃で2時間焼成して、ハニカム構造の珪素−炭化珪素多孔体を得た。それ以外は、実施例1と同様にして焼結体を作製し(作製条件を表2に示す)、試験片を切出した。実施例1と同様にして、上記の評価項目の測定を行った。測定結果を表4に示す。
実施例1において炭化珪素(SiC)の平均粒径を24μmとし、実施例1の「成形体の窒化前焼成」において、常圧(大気圧)、アルゴン雰囲気(酸素分圧100Pa)中、1450℃で2時間焼成して、ハニカム構造の珪素−炭化珪素多孔体を得た。それ以外は、実施例1と同様にして焼結体を作製し(作製条件を表2に示す)、試験片を切出した。実施例1と同様にして、上記の評価項目の測定を行った。測定結果を表4に示す。
助剤(実施例1においては、炭酸ストロンチウム)の添加量を3質量%とし、実施例1において、「ハニカム構造の珪素−炭化珪素多孔体を、常圧(大気圧)、窒素雰囲気で1450℃で4時間保持し、更に1750℃で4時間保持」した「窒化時焼成条件」を、「ハニカム構造の珪素−炭化珪素多孔体を、常圧(大気圧)、窒素雰囲気で1100℃で12時間保持」することとした。その他の条件は、実施例1と同様にした。また、実施例1と同様にして、得られた焼結体から試験片を切出し、上記の評価項目の測定を行った。測定結果を表4に示す。
Claims (11)
- 骨材としての炭化珪素粒子が、窒化珪素を結合材として、前記炭化珪素粒子相互間に細孔を保持した状態で結合してなる多孔質材料であって、
前記細孔内の前記窒化珪素表面に柱状体(窒化珪素ウィスカー)が存在しないか、又は不可避的に存在するとしても、太さが2μmより大きく且つアスペクト比が10より小さい柱状体の数が、太さが2μm以下またはアスペクト比が10以上である柱状体の数よりも多いことを特徴とする多孔質材料。 - 骨材としての炭化珪素粒子が、窒化珪素を結合材として、前記炭化珪素粒子相互間に細孔を保持した状態で結合してなる多孔質材料であって、
前記細孔の比表面積が1m2/g以下であることを特徴とする請求項1に記載の多孔質材料。 - 前記細孔の開気孔率が40〜75%である請求項1又は2に記載の多孔質材料。
- 前記細孔の平均細孔径が5〜50μmである請求項1〜3のいずれかに記載の多孔質材料。
- 耐熱温度が1200℃以上である請求項1〜4のいずれかに記載の多孔質材料。
- ガス透過係数が1μm2以上である請求項1〜5のいずれかに記載の多孔質材料。
- 請求項1〜6のいずれかに記載の多孔質材料の製造方法であって、少なくとも珪素、炭化珪素及び造孔剤を混合し、酸素分圧が10Pa以下となるような、不活性ガス雰囲気下又は減圧雰囲気下、1400〜1500℃で焼成して珪素−炭化珪素多孔体を作製し、得られた前記珪素−炭化珪素多孔体を窒素雰囲気下で1200〜1800℃で窒化及び焼成することを特徴とする多孔質材料の製造方法。
- 前記珪素−炭化珪素多孔体を作製した後、室温まで降温することなく1200℃以上の温度を維持しながら窒素雰囲気へ切り換えて、前記窒化珪素−炭化珪素多孔体を前記窒素雰囲気下で1200〜1800℃で窒化及び焼成する請求項7に記載の多孔質材料の製造方法。
- 前記珪素−炭化珪素多孔体を作製した後、水素を0.1体積%以上混合した窒素雰囲気下で1200〜1800℃で窒化及び焼成する請求項7に記載の多孔質材料の製造方法。
- 前記珪素−炭化珪素多孔体を作製した後、室温まで降温することなく1200℃以上の温度を維持しながら水素を0.1体積%以上混合した窒素雰囲気(水素混合窒素雰囲気)へ切り換えて、前記珪素−炭化珪素多孔体を前記水素混合窒素雰囲気下で1200〜1800℃で窒化及び焼成する請求項7に記載の多孔質材料の製造方法。
- 請求項1〜6のいずれかに記載の多孔質材料から構成されたハニカム構造体。
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JP2507151B2 (ja) * | 1990-06-29 | 1996-06-12 | シャープ株式会社 | 導電性セラミックス焼結体及びその製造方法 |
JP3099195B2 (ja) * | 1990-08-10 | 2000-10-16 | 東海高熱工業株式会社 | 窒化けい素結合炭化けい素質担体及びその製造方法 |
JP2732708B2 (ja) * | 1990-09-21 | 1998-03-30 | シャープ株式会社 | 導電性セラミック焼結体 |
WO1994008915A1 (de) * | 1992-10-22 | 1994-04-28 | H.C. STARCK G.M.B.H. & Co. KG. | VERFAHREN ZUR HERSTELLUNG FEUERFESTER FORMKÖRPER AUF SiC-BASIS MIT SILICIUMNITRID/-OXINITRIDBINDUNG, IHRE VERWENDUNG, SOWIE PRESSMASSE ALS ZWISCHENPRODUKT |
JP2801821B2 (ja) * | 1992-10-30 | 1998-09-21 | 京セラ株式会社 | セラミック複合焼結体およびその製造方法 |
JP2002530175A (ja) * | 1998-11-20 | 2002-09-17 | コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ | コードレス走査ヘッドの充電器を備える超音波診断イメージングシステム |
DE60025989T2 (de) * | 1999-04-09 | 2006-11-09 | Tosoh Corp., Shinnanyo | Formschleifprodukt und Benutzung in einer Polierscheibe |
JP3965007B2 (ja) * | 1999-09-29 | 2007-08-22 | イビデン株式会社 | 多孔質炭化珪素焼結体、ハニカムフィルタ、セラミックフィルタ集合体 |
EP1770142A3 (en) * | 2000-10-06 | 2008-05-07 | 3M Innovative Properties Company | A method of making agglomerate abrasive grain |
JP2002274947A (ja) * | 2001-03-16 | 2002-09-25 | Ibiden Co Ltd | 多孔質炭化珪素焼結体及びその製造方法、ディーゼルパティキュレートフィルタ |
US6699429B2 (en) * | 2001-08-24 | 2004-03-02 | Corning Incorporated | Method of making silicon nitride-bonded silicon carbide honeycomb filters |
-
2004
- 2004-03-19 EP EP20040722013 patent/EP1634859B1/en not_active Expired - Lifetime
- 2004-03-19 PL PL04722013T patent/PL1634859T3/pl unknown
- 2004-03-19 KR KR1020057017593A patent/KR100666426B1/ko not_active IP Right Cessation
- 2004-03-19 US US10/549,762 patent/US20060175741A1/en not_active Abandoned
- 2004-03-19 JP JP2005503755A patent/JP4426525B2/ja not_active Expired - Lifetime
- 2004-03-19 WO PCT/JP2004/003738 patent/WO2004083148A1/ja active Application Filing
Also Published As
Publication number | Publication date |
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KR100666426B1 (ko) | 2007-01-11 |
EP1634859B1 (en) | 2013-06-19 |
KR20050122212A (ko) | 2005-12-28 |
US20060175741A1 (en) | 2006-08-10 |
EP1634859A4 (en) | 2008-11-26 |
WO2004083148A1 (ja) | 2004-09-30 |
PL1634859T3 (pl) | 2013-11-29 |
JPWO2004083148A1 (ja) | 2006-06-22 |
EP1634859A1 (en) | 2006-03-15 |
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