JP4683554B2 - 多孔質チタニア成形体の製造方法 - Google Patents
多孔質チタニア成形体の製造方法 Download PDFInfo
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- JP4683554B2 JP4683554B2 JP2005515801A JP2005515801A JP4683554B2 JP 4683554 B2 JP4683554 B2 JP 4683554B2 JP 2005515801 A JP2005515801 A JP 2005515801A JP 2005515801 A JP2005515801 A JP 2005515801A JP 4683554 B2 JP4683554 B2 JP 4683554B2
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
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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
- C04B35/46—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 titanium oxides or titanates
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
Description
本発明において、無機粒子のゾルを出発原料とする。
共連続構造は、相分離によるドメイン形成とゾルゲル転移が並行して起こるときに得られる。これに対して、ゾルゲル転移が相分離よりも早く起こった場合には、均一ゲル組成が得られる。また、相分離がゾルゲル転移よりも早く起こった場合には、巨視的二相分離が起こる。本発明においては、ゾルゲル転移と相分離との進行の早さを調整することによって、均一ゲル組成と巨視的二層分離との中間にある過渡的なネットワーク構造(共連続構造)を生じさせ、そのまま固定して多孔質成形体を得ることに成功した。
また、中心細孔径の±20%に、0.1μm以上のマクロ孔全体の50%以上が存在することを特徴とする、チタニア多孔質体を提供できる。
本発明においては、ゾルを強酸性とし、このゾルのpHを増加させることによってチタニア粒子の凝集および相分離を進行させる。ゾルを強酸性とすることによって、粒子間の静電的反発を大きくし、粒子を均一に分散させることができる。これによって、いっそう均一な孔分布を有する多孔質成形体が得られる。
保持部材の間隙に面する内壁面のRaを測定するためには、保持部材を切断し、間隙に面する内壁面を露出させる。次いで、内壁面のRaを表面粗さ計によって測定する。
(試料の作製)
表1のチタニア粒子を出発原料とし、表2〜4の各例に示す各試料を作製した。
具体的には、試薬として、分子量10万のポリエチレンオキシド(アルドリッチ社製)、60%濃硝酸(林純薬工業株式会社製、特級)、チタニアゾル(石原産業製、STS−010)、ホルムアミドを用いた。ポリエチレンオキシドを硝酸溶液に溶解し、氷冷下、チタニアゾル、ホルムアミドを加え、攪拌し、均一なゾルを得た。ゾルを容器に入れ、容器を密封し、40℃恒温槽にてゲル化、24時間エージングを行った。その後、2−メチル−2−プロパノールを用いて溶媒置換し、凍結乾燥した。得られた成形体を1200℃で1時間熱処理し、焼結体とした。
熱処理前後の試料のモルフォロジーの観察は、走査型電子顕微鏡(SEM:日立製作所製S−510型)を用いた。モルフォロジーの区別は、連続したチタニア骨格とマイクロメートル領域に連続した貫通孔を持つものを「共連続構造あり」とし、マイクロメートル領域に細孔が見られなかったものを「マクロ孔なし」とした。
熱処理前後の試料の結晶性の同定を、理学電気製「RAD-Cシステム」を用い、X線回折測定(CuKa線)により行なった。試料をメノウ乳鉢を用いて微細な粉末にして行なった。得られたピークの積分値を用いてScherrerの式により、結晶子のサイズを求めた。lはX線の波長、B(2q)は回折線幅、qは回折角、Kは定数でB(2q)に半値幅を用いた場合K=0.9となる。
ランダム媒質の光学特性評価として、後方散乱測定を行った。平行光を入射すると、ちょうど逆向きに出て行く光と干渉する確率が一番高く、ほかの角度よりも散乱強度が大きくなる。光を強く散乱する媒体を用いると、光の局在化が起こり、周辺の角度でも大きな散乱強度が得られる。一回の散乱で光が進む距離を表す光の平均自由行程l が光の波長程度となるとき、光は最も局在化する。
後方散乱における散乱強度について(式1)
を用いて理論的に計算すると、光の平均自由行程が光の波長程度になると最もピークの幅が広がり、強く光を局在化していると考えられる。ローダミン色素レーザー(l=488nm)を照射し散乱強度を測定した。色素レーザーの励起にはCWのAr+レーザーを用いた。測定結果より式1を用いて光の平均自由行程を求めた。
図5(番号2−4)では、ゲル化に対して相分離のタイミングが遅れたために、マクロ孔なしの構造が得られた。図6〜8(番号2−1、2−2、2−3)では、共連続構造が得られた。この中でも、チタニアに対するポリエチレンオキシドの量が増えるに従い、ゲル化に対して相分離のタイミングが早まり、ドメインサイズが大きくなる。これより、ポリエチレンオキシドの量によって相分離傾向を変化させ、細孔径を制御できると考えられる。
図15(c)に模式的に示すようなハニカム構造体2Cの空隙4C内に多孔質成形体3Cを形成させた。具体的には、ハニカム構造体2Cのセルピッチ1.05mm、壁厚0.1mm、面間隔(間隙の幅m)0.95mm、壁面の気孔率約30%とした。
Claims (3)
- チタニア粒子、水、水溶性の高分子あるいは界面活性物質、酸、および有機アミドを含む強酸性ゾルにおいて、前記チタニア粒子の重量を100重量部としたときに前記水溶性の高分子あるいは界面活性物質の添加量が3重量部以上であり、前記有機アミドの添加量が10重量部以上であり、経時により前記ゾルのpHを増加させることによって前記チタニア粒子の凝集および相分離を同時に進行させ、前記相分離後に、前記水を乾燥によって除去する、開気孔を含む多孔質チタニア成形体を製造する方法。
- 前記有機アミドがホルムアミドであることを特徴とする、請求項1記載の方法。
- 請求項1または2記載の前記成形体を熱処理することによって多孔質焼結体を製造する方法。
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JP2005515801A JP4683554B2 (ja) | 2003-11-28 | 2004-11-18 | 多孔質チタニア成形体の製造方法 |
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JP2003398869 | 2003-11-28 | ||
JP2003398869 | 2003-11-28 | ||
JP2005515801A JP4683554B2 (ja) | 2003-11-28 | 2004-11-18 | 多孔質チタニア成形体の製造方法 |
PCT/JP2004/017523 WO2005051864A1 (ja) | 2003-11-28 | 2004-11-18 | 多孔質成形体、多孔質焼結体、その製造方法及びその複合部材 |
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JPWO2005051864A1 JPWO2005051864A1 (ja) | 2007-06-21 |
JP4683554B2 true JP4683554B2 (ja) | 2011-05-18 |
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Country | Link |
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US (1) | US20060204764A1 (ja) |
EP (1) | EP1688402A4 (ja) |
JP (1) | JP4683554B2 (ja) |
CN (1) | CN1852874A (ja) |
WO (1) | WO2005051864A1 (ja) |
Families Citing this family (19)
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JP4874976B2 (ja) * | 2005-08-19 | 2012-02-15 | 国立大学法人京都大学 | 無機系多孔質体及びその製造方法 |
SG175681A1 (en) | 2006-10-25 | 2011-11-28 | Proteus Biomedical Inc | Controlled activation ingestible identifier |
CA2676407A1 (en) | 2007-02-01 | 2008-08-07 | Proteus Biomedical, Inc. | Ingestible event marker systems |
CN101636865B (zh) | 2007-02-14 | 2012-09-05 | 普罗秋斯生物医学公司 | 具有高表面积电极的体内电源 |
US8540632B2 (en) | 2007-05-24 | 2013-09-24 | Proteus Digital Health, Inc. | Low profile antenna for in body device |
SG10201702853UA (en) | 2008-07-08 | 2017-06-29 | Proteus Digital Health Inc | Ingestible event marker data framework |
US8278231B2 (en) * | 2008-11-24 | 2012-10-02 | Exxonmobil Chemical Patents Inc. | Heat stable formed ceramic, apparatus and method of using the same |
TWI517050B (zh) | 2009-11-04 | 2016-01-11 | 普羅托斯數位健康公司 | 供應鏈管理之系統 |
TWI557672B (zh) | 2010-05-19 | 2016-11-11 | 波提亞斯數位康健公司 | 用於從製造商跟蹤藥物直到患者之電腦系統及電腦實施之方法、用於確認將藥物給予患者的設備及方法、患者介面裝置 |
WO2015112603A1 (en) | 2014-01-21 | 2015-07-30 | Proteus Digital Health, Inc. | Masticable ingestible product and communication system therefor |
CN103827914A (zh) | 2011-07-21 | 2014-05-28 | 普罗秋斯数字健康公司 | 移动通信设备、系统和方法 |
JP5846056B2 (ja) * | 2012-06-28 | 2016-01-20 | 株式会社豊田自動織機 | セパレータの製造方法 |
JP6511439B2 (ja) | 2013-06-04 | 2019-05-15 | プロテウス デジタル ヘルス, インコーポレイテッド | データ収集および転帰の査定のためのシステム、装置、および方法 |
KR102051875B1 (ko) | 2016-07-22 | 2019-12-04 | 프로테우스 디지털 헬스, 인코포레이티드 | 섭취 가능한 이벤트 마커의 전자기 감지 및 검출 |
CN106395896B (zh) * | 2016-11-30 | 2018-01-05 | 浙江理工大学 | 一种微孔球状二氧化钛的制备方法 |
KR102079734B1 (ko) | 2017-01-26 | 2020-02-20 | 주식회사 엘지화학 | 산화적 탈수소화 반응용 페라이트 촉매, 이의 제조방법 및 이를 이용한 부타디엔의 제조방법 |
CN110937880A (zh) * | 2018-09-25 | 2020-03-31 | 中国石油化工股份有限公司 | 一种整体式氧化铝材料及其制备方法 |
CN109759594B (zh) | 2019-01-08 | 2020-09-11 | 钢铁研究总院 | 一种组合材料热等静压高通量微制造方法及其包套模具 |
CN114433041B (zh) * | 2020-10-30 | 2024-03-08 | 中国石油化工股份有限公司 | 一种超大孔氧化铝材料及其制备方法 |
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EP1270202B1 (en) * | 1996-01-12 | 2006-04-26 | Ibiden Co., Ltd. | Filter for purifying exhaust gas |
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2004
- 2004-11-18 CN CNA2004800266175A patent/CN1852874A/zh active Pending
- 2004-11-18 EP EP04799812A patent/EP1688402A4/en not_active Withdrawn
- 2004-11-18 JP JP2005515801A patent/JP4683554B2/ja active Active
- 2004-11-18 WO PCT/JP2004/017523 patent/WO2005051864A1/ja not_active Application Discontinuation
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2006
- 2006-03-13 US US11/375,603 patent/US20060204764A1/en not_active Abandoned
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JPH0558649A (ja) * | 1991-09-02 | 1993-03-09 | Tokuyama Soda Co Ltd | シリカ−チタニアガラスの製造方法 |
JPH0828246A (ja) * | 1994-07-14 | 1996-01-30 | Ibiden Co Ltd | セラミック構造体 |
JPH10182260A (ja) * | 1996-12-26 | 1998-07-07 | Naohiro Soga | 無機系多孔質体の製造方法 |
JPH1161209A (ja) * | 1997-08-15 | 1999-03-05 | Kdk Corp | 貴金属微粒子の分散体及びその製造方法、並びに分散体を利用した構造体デバイス及びその製造方法 |
JPH11292528A (ja) * | 1998-01-23 | 1999-10-26 | Naohiro Soga | 無機多孔質材料の製造法 |
JPH11292520A (ja) * | 1998-04-14 | 1999-10-26 | Showa Denko Kk | 表面フッ素化金属酸化物ゾル及びその製造方法 |
JP2001162119A (ja) * | 1999-09-29 | 2001-06-19 | Ibiden Co Ltd | セラミックフィルタ集合体 |
JP2002293657A (ja) * | 2001-04-02 | 2002-10-09 | Naohiro Soga | 分散粒子を含む無機系多孔質複合体の製造方法 |
WO2004031101A1 (ja) * | 2002-10-07 | 2004-04-15 | Ibiden Co., Ltd. | ハニカム構造体 |
WO2005042402A1 (ja) * | 2003-10-31 | 2005-05-12 | Ngk Insulators, Ltd. | 分散粒子を含む無機系多孔質体 |
WO2005046834A1 (de) * | 2003-11-06 | 2005-05-26 | Merck Patent Gmbh | Verfahren zur herstellung von monolithischen formkörpern |
Also Published As
Publication number | Publication date |
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CN1852874A (zh) | 2006-10-25 |
EP1688402A4 (en) | 2010-07-07 |
JPWO2005051864A1 (ja) | 2007-06-21 |
US20060204764A1 (en) | 2006-09-14 |
WO2005051864A1 (ja) | 2005-06-09 |
EP1688402A1 (en) | 2006-08-09 |
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