JP5478243B2 - 接合材組成物及びその製造方法並びに接合体及びその製造方法 - Google Patents
接合材組成物及びその製造方法並びに接合体及びその製造方法 Download PDFInfo
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- JP5478243B2 JP5478243B2 JP2009506253A JP2009506253A JP5478243B2 JP 5478243 B2 JP5478243 B2 JP 5478243B2 JP 2009506253 A JP2009506253 A JP 2009506253A JP 2009506253 A JP2009506253 A JP 2009506253A JP 5478243 B2 JP5478243 B2 JP 5478243B2
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- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
- F01N3/0222—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous the structure being monolithic, e.g. honeycombs
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Description
(ハニカムセグメント(被接合物)の作製)
ハニカムセグメント原料として、SiC粉末及び金属Si粉末を80:20の質量割合で混合し、これに造孔材、有機バインダー、界面活性剤及び水を添加して、可塑性の坏土を作製した。この坏土を押出成形し、乾燥して隔壁の厚さが310μm、セル密度が約46.5セル/cm2(300セル/平方インチ)、断面が一辺35mmの正四角形、長さが152mmのハニカムセグメント成形体を得た。次いで、このハニカムセグメント成形体の端面が市松模様状を呈するように、各セルの一方の端部を目封止した。すなわち、隣接するセルが、互いに反対側の端部で封じられるように目封止を行った。目封止用の充填材には、ハニカムセグメント原料と同様の材料を用いた。こうしてセルを目封止し、乾燥させた後、大気雰囲気中約400℃で脱脂し、その後、Ar不活性雰囲気にて約1450℃で焼成して、SiC結晶粒子をSiで結合させた、多孔質構造を有するハニカムセグメントを得た。
表1に示す条件で、板状粒子A(平均粒径50μm未満)、板状粒子B(平均粒径50μm以上)、非板状粒子、有機バインダー、発泡樹脂を混合したものに、無機接着剤、分散剤、水を更に混合し、ミキサーにて30分間混練を行い、組成の異なるペースト状の接合材組成物(接合材組成物No.1〜26)をそれぞれ得た。このとき、ペースト状の接合材組成物の粘度が20〜60Pa・sとなるように水の添加量を調整した。なお、接合材組成物No.7で板状粒子として用いた仮焼タルクは900℃で仮焼したものであり、接合材組成物No.8で板状粒子として用いた仮焼マイカは800℃で仮焼したものである。主成分である、板状粒子A、板状粒子B、非板状粒子、無機接着剤の割合は、これらの合計を100としたときの、それぞれの質量%で表示した。また、副成分である、有機バインダー、発泡樹脂、分散剤の割合は、主成分を100としたときの外配の質量%で表示した。板状粒子Aと板状粒子Bのアスペクト比は、当該粒子の「長径/厚さ」として算出され、前記「長径」及び「厚さ」の測定は、電子顕微鏡観察により行った。すなわち、板状粒子の厚さ方向に垂直な任意の方向から観察し、その電子顕微鏡写真を画像処理することにより、厚さを計測した。また、同じ画像において、厚さ方向に垂直な方向の粒子の長さを長径とし、画像処理により長径を計測した。なお、この計測は、観察視野中から無作為に選択した10ヶ以上の粒子について実施し、それらのアスペクト比の平均値を板状粒子のアスペクト比とした。
ハニカムセグメントの外壁面に、厚さ約1mmとなるように接合材組成物No.1を塗布方向をハニカムセグメントの長手方向としてコーティングして接合材層を形成し、その上に別のハニカムセグメントを載置する工程を繰り返し、縦4個×横4個に組み合わせた合計16個のハニカムセグメントからなるハニカムセグメント積層体を作製し、適宜、外部より圧力を加えるなどして、全体を接合させた後、140℃で2時間乾燥してハニカムセグメント接合体を得た。得られたハニカムセグメント接合体の外周を円筒状に研削加工後、その外周面をコーティング材で被覆し、700℃で2時間乾燥硬化させて、ハニカム構造体を得た。
得られたハニカム構造体の接合材層について、気孔率、被接合物のヤング率に対する接合材層の厚さ方向の圧縮ヤング率の割合、接合体の接合曲げ試験における曲げ強度を、下記の方法により求めた。その結果を表2に示す。
ハニカム構造体から接合材層の部分を任意形状に切り出し(例えば、10×10×1mmの板状)、アルキメデス法により算出した。
ハニカム構造体から接合材層の部分を所定の形状に切り出し(例えば、10×10×1mmの板状)、切り出した試験片に対して所定の圧縮荷重を負荷したときの変位を計測し、その応力−歪線図から算出した(被接合物のヤング率は、JIS R1601に準じた3点曲げ試験における荷重−変位曲線から算出した。)。
JIS R1624に準じて、二つの被接合物と接合材層とからなる接合体の試験片(例えば、10×15×70mm)を切り出し、曲げ試験での強度を測定した。
得られたハニカム構造体の接合後の状態を確認するとともに、下記の方法により、急速加熱試験(バーナースポーリング試験)を試験温度900℃、1000℃にて行った。試験後のハニカム構造体のクラックの発生状況を観察した。その結果を表3に示す。
ハニカム構造体にバーナーで加熱した空気を流すことにより中心部分と外側部分との温度差をつくり、ハニカム構造体のクラックの発生しない温度により耐熱衝撃性を評価する試験(温度が高いほど耐熱衝撃性が高い)である。なお、表3の表示では、×の場合、試験温度900℃でクラック発生あり、○の場合、試験温度900℃でクラック発生なし、◎の場合、試験温度1000℃でクラック発生なしを意味する。
実施例2〜22は、実施例1において、接合材組成物No.1を、表1に示す接合材組成物No.2〜22に変えたこと以外、実施例1と同様に、ハニカム構造体を作製した。また、比較例1〜4は、接合材組成物No.23〜26に変えたこと以外は実施例1と同様に、ハニカム構造体を作製した。それぞれ得られたハニカム構造体(実施例2〜22、比較例1〜4)について、実施例1と同様の評価及び試験を行った。その結果を表2及び表3に示す。
表2及び表3の結果から、本発明の実施例に係る実施例1〜22は、硬化後の接合材組成物(接合材層)の評価が良好であり、ハニカムセグメント間の接合状態も良好であり、かつ、試験温度900℃での急速加熱試験後であっても、ハニカム構造体の端部、外周部及び接合材層にクラックが発生することなく、良品であった。一方、フィラーとして板状粒子の代わりにファイバーを含む接合材組成物を使用した比較例1は、急速加熱試験後のハニカム構造体の端部にクラックが生じた。また、フィラーとして板状粒子を含まない接合材組成物を使用した比較例2は、十分な高気孔率化が行えず、被接合物のヤング率に対する接合材層の厚さ方向の圧縮ヤング率の割合が大きくなり、急速加熱試験後のハニカム構造体の外周部及び接合材層にクラックが生じた。更に、板状粒子の割合が主成分全体の30質量%未満である接合材組成物を使用した比較例3と、板状粒子の割合が主成分全体の50質量%超である接合材組成物を使用した比較例4は、接合曲げ試験における曲げ強度が低く、急速加熱試験後のハニカム構造体の外周部及び接合材層にクラックが生じた。
Claims (20)
- 二つ以上の被接合物が接合材層を介して一体化されてなる接合体を得るための接合材組成物であって、板状粒子、非板状粒子及び無機接着剤を主成分とし、前記板状粒子の割合が前記主成分全体の30〜50質量%であり、前記板状粒子のアスペクト比が3以上であり、前記非板状粒子の平均粒径が10μm未満である接合材組成物。
- 前記板状粒子が、平均粒径50μm未満の板状粒子Aと平均粒径50μm以上の板状粒子Bとからなる請求項1に記載の接合材組成物。
- 前記板状粒子が、マイカ、タルク、窒化ホウ素及びガラスフレークよりなる群から選ばれた1種以上の材料からなる板状粒子である請求項1又は2に記載の接合材組成物。
- 前記マイカが800℃以上で仮焼したマイカであり、前記タルクが900℃以上で仮焼したタルクである請求項3に記載の接合材組成物。
- 前記非板状粒子が、アルミナ、シリカ、ムライト、ジルコニア、炭化珪素、窒化珪素、窒化アルミニウム及びガラスよりなる群から選ばれた1種以上の材料からなる非板状粒子である請求項1〜4の何れか一項に記載の接合材組成物。
- 前記無機接着剤が、コロイダルシリカである請求項1〜5の何れか一項に記載の接合材組成物。
- 前記接合材組成物の副成分として、有機バインダー、分散剤、発泡樹脂及び水を含む請求項1〜6の何れか一項に記載の接合材組成物。
- 前記有機バインダーとして、メチルセルロースを含む請求項7に記載の接合材組成物。
- 前記接合材組成物に含まれる前記発泡樹脂の割合が、前記主成分全体に対し、外配で0.1〜5.0質量%である請求項7又は8に記載の接合材組成物。
- 前記被接合物が、ハニカムセグメントである請求項1〜9の何れか一項に記載の接合材組成物。
- 前記ハニカムセグメントが、ディーゼル排ガス浄化用フィルターに使用するハニカム構造体を得るためのハニカムセグメントである請求項10に記載の接合材組成物。
- 二つ以上の被接合物が、請求項1〜11の何れか一項に記載の接合材組成物によって形成される接合材層を介して一体化されてなる接合体であって、前記接合材層の気孔率が60〜80%である接合体。
- 前記接合材層の厚さ方向の圧縮ヤング率が、前記被接合物のヤング率の5%以下である請求項12に記載の接合体。
- 二つの被接合物とそれらを接合している接合材層とを試験片として切り出し、接合曲げ試験に供した場合における曲げ強度が、0.2MPa以上である請求項12又は13に記載の接合体。
- 前記被接合物が、ハニカムセグメントである請求項12〜14の何れか一項に記載の接合体。
- ディーゼル排ガス浄化用フィルターに使用される請求項12〜15の何れか一項に記載の接合体。
- 主成分としてアスペクト比が3以上の板状粒子、平均粒径10μm未満の非板状粒子及び無機接着剤が含まれ、前記板状粒子の割合が、前記主成分全体の30〜50質量%である原料を、混合、混練してペースト状にする接合材組成物の製造方法。
- 前記原料に、更に副成分として有機バインダー、分散剤、発泡樹脂及び水が含まれる請求項17に記載の接合材組成物の製造方法。
- 二つ以上の被接合物を、請求項1〜11の何れか一項に記載の接合材組成物を用いて一体的に接合する接合体の製造方法。
- 前記被接合物がハニカムセグメントである、請求項19に記載の接合体の製造方法。
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JP5244619B2 (ja) * | 2007-02-08 | 2013-07-24 | 日本碍子株式会社 | 接合材組成物及びその製造方法並びに接合体及びその製造方法 |
KR20120095960A (ko) * | 2009-11-11 | 2012-08-29 | 다우 글로벌 테크놀로지스 엘엘씨 | 내열충격성 세라믹 허니컴 구조물 제조를 위한 개선된 시멘트 및 이의 제조방법 |
GB201105957D0 (en) | 2011-04-08 | 2011-05-18 | Element Six Ltd | Containment element |
JP6423160B2 (ja) | 2014-03-04 | 2018-11-14 | 日本碍子株式会社 | ハニカム構造体 |
JP6077484B2 (ja) | 2014-03-26 | 2017-02-08 | 日本碍子株式会社 | ハニカム構造体 |
EP3202477B1 (en) | 2014-09-30 | 2020-03-11 | Hitachi Metals, Ltd. | Ceramic honeycomb filter and method for manufacturing same |
GB201721306D0 (en) | 2017-12-19 | 2018-01-31 | Knauf Insulation Ltd | Mineral fiber based composites |
JPWO2022138906A1 (ja) * | 2020-12-25 | 2022-06-30 |
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- 2008-02-26 EP EP08711974.9A patent/EP2138475B1/en not_active Not-in-force
- 2008-02-26 WO PCT/JP2008/053245 patent/WO2008117611A1/ja active Application Filing
- 2008-02-26 JP JP2009506253A patent/JP5478243B2/ja not_active Expired - Fee Related
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JPWO2008117611A1 (ja) | 2010-07-15 |
WO2008117611A1 (ja) | 2008-10-02 |
EP2138475A4 (en) | 2014-04-30 |
EP2138475B1 (en) | 2018-10-03 |
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