JP5176198B2 - マクロポーラスな連通孔を持つセラミック多孔体の製造方法 - Google Patents
マクロポーラスな連通孔を持つセラミック多孔体の製造方法 Download PDFInfo
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- JP5176198B2 JP5176198B2 JP2007041513A JP2007041513A JP5176198B2 JP 5176198 B2 JP5176198 B2 JP 5176198B2 JP 2007041513 A JP2007041513 A JP 2007041513A JP 2007041513 A JP2007041513 A JP 2007041513A JP 5176198 B2 JP5176198 B2 JP 5176198B2
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- porous body
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- 239000000919 ceramic Substances 0.000 title claims description 96
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 238000004891 communication Methods 0.000 title claims description 11
- 239000011148 porous material Substances 0.000 claims description 55
- 238000001035 drying Methods 0.000 claims description 46
- 239000002002 slurry Substances 0.000 claims description 41
- 230000008014 freezing Effects 0.000 claims description 33
- 238000007710 freezing Methods 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229920003169 water-soluble polymer Polymers 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 16
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 229920000642 polymer Polymers 0.000 claims description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 229910052878 cordierite Inorganic materials 0.000 claims description 4
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 4
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- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 3
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 229910052586 apatite Inorganic materials 0.000 description 2
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- 239000002781 deodorant agent Substances 0.000 description 2
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- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 2
- 229910021426 porous silicon Inorganic materials 0.000 description 2
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
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- 241000287463 Phalacrocorax Species 0.000 description 1
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- 239000011358 absorbing material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
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- 239000003505 polymerization initiator Substances 0.000 description 1
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Classifications
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- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/007—Producing shaped prefabricated articles from the material by freezing the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
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- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
- C04B38/062—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles the burned-out substance being formed in situ, e.g. by polymerisation of a prepolymer composition containing ceramic powder
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- C04B2103/44—Thickening, gelling or viscosity increasing agents
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- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Description
(1)ゲル化可能な水溶性高分子の水溶液にセラミック粉体を分散したスラリーをゲル化させ、凍結、乾燥、焼結して、セラミック多孔体を製造する方法であって、
その際に、1)上記ゲル化可能な水溶性高分子として、N−アルキルアクリルアミド系高分子、N−イソプロピルアクリルアミド系高分子、スルホメチル化アクリルアミド系高分子、N−ジメチルアミノプロピルメタクリルアミド系高分子、ポリアルキルアクリルアミド系高分子、アルギン酸、ポリエチレンイミン、でんぷん、カルボシキメチルセルロース、ゼラチン、ヒドロシキメチルセルロース、ポリアクリル酸ナトリウム、ポリビニルアルコール、ポリエチレングリコール、寒天、又はポリエチレンオキシドを用い、2)上記セラミック粉体として、平均粒径0.01μm〜5μmのセラミック粉体を使用し、3)上記乾燥工程において、凍結体を真空乾燥、あるいは水溶性有機溶媒中への浸漬と風乾により、氷を気孔に置換してゆく乾燥法により乾燥し、亀裂の無い成形体を得ることにより、
平均気孔径10μm〜300μmのマクロポーラスな連通孔を有し、気孔率が72%〜99%であるセラミック多孔体を作製することを特徴とするセラミック多孔体の製造方法。
(2)セラミック粉体を分散したスラリーとして、セラミック粉体の固形分濃度が1vol%〜28vol%のスラリーを用いる、前記(1)に記載のセラミック多孔体の製造方法。
(3)セラミック原料として、アルミナ、ジルコニア、炭化珪素、窒化珪素、コーディエライト、又はハイドロキシアパタイトを用いる、前記(1)に記載のセラミック多孔体の製造方法。
(4)ゲル化させたスラリーを、−10℃より低い凍結温度で凍結させる、前記(1)に記載のセラミック多孔体の製造方法。
(5)凍結体を水溶性有機溶媒に浸漬して水と有機溶媒の置換を行う操作を複数回繰り返すことにより、凍結体中の氷であった部分を有機溶媒に置換する、前記(1)に記載のセラミック多孔体の製造方法。
本発明は、ゲル化可能な水溶性高分子の水溶液にセラミック粉体を分散したスラリーを、ゲル化、凍結、解凍、乾燥、焼結してセラミック多孔体を製造する方法であって、0.01μm〜5μmのセラミック粉体を使用し、スラリーのゲル化及び凍結で、高分子から放出された水の凍結によって発達した氷の結晶による組織構造を有する凍結体を形成し、これを解凍、乾燥、焼結工程で壊すことなく保持して、これまで作製が困難であった10μm〜300μmのマクロポーラスな連通孔を持ち、72%〜99%の高気孔率を有するセラミック多孔体を作製することを特徴とするものである。図1に、本発明によるセラミック多孔体の製造方法の概念を示す。
(1)氷の結晶組織をそのまま空間に置換した、粗大な気孔径、連続する気孔及び様々な気孔形状からなる、10μm〜300μmのマクロポーラスな連通孔を有し、気孔率が72%〜99%で、0.4MPa以上の圧縮強度を有することで特徴付けられるセラミック多孔体を提供することができる。
(2)従来法で作製することが困難であった、72%以上の高気孔率で、しかも強度の高いセラミック多孔体である、アルミナ、ジルコニア、炭化珪素、窒化珪素、コーディエライト、ハイドロキシアパタイトの多孔体を提供することができる。
(3)ゲル凍結法と「雰囲気制御置換型乾燥法」を用いた解凍方法を組み合せることで、上記セラミック多孔体を製造することが実現できる。
(4)本発明の製造方法で得られるセラミック多孔体は、例えば、フィルター、吸湿、吸水、吸音材、吸着材、消臭剤、生活健康資材、散気板、リアクター、衝撃吸収材、軽量材、触媒担体、固体触媒、断熱材、耐火物、生体材料、真空チャック、電磁波遮断材等、汎用的な用途に幅広く応用可能である。
Claims (5)
- ゲル化可能な水溶性高分子の水溶液にセラミック粉体を分散したスラリーをゲル化させ、凍結、乾燥、焼結して、セラミック多孔体を製造する方法であって、
その際に、1)上記ゲル化可能な水溶性高分子として、N−アルキルアクリルアミド系高分子、N−イソプロピルアクリルアミド系高分子、スルホメチル化アクリルアミド系高分子、N−ジメチルアミノプロピルメタクリルアミド系高分子、ポリアルキルアクリルアミド系高分子、アルギン酸、ポリエチレンイミン、でんぷん、カルボシキメチルセルロース、ゼラチン、ヒドロシキメチルセルロース、ポリアクリル酸ナトリウム、ポリビニルアルコール、ポリエチレングリコール、寒天、又はポリエチレンオキシドを用い、2)上記セラミック粉体として、平均粒径0.01μm〜5μmのセラミック粉体を使用し、3)上記乾燥工程において、凍結体を真空乾燥、あるいは水溶性有機溶媒中への浸漬と風乾により、氷を気孔に置換してゆく乾燥法により乾燥し、亀裂の無い成形体を得ることにより、
平均気孔径10μm〜300μmのマクロポーラスな連通孔を有し、気孔率が72%〜99%であるセラミック多孔体を作製することを特徴とするセラミック多孔体の製造方法。 - セラミック粉体を分散したスラリーとして、セラミック粉体の固形分濃度が1vol%〜28vol%のスラリーを用いる、請求項1に記載のセラミック多孔体の製造方法。
- セラミック原料として、アルミナ、ジルコニア、炭化珪素、窒化珪素、コーディエライト、又はハイドロキシアパタイトを用いる、請求項1に記載のセラミック多孔体の製造方法。
- ゲル化させたスラリーを、−10℃より低い凍結温度で凍結させる、請求項1に記載のセラミック多孔体の製造方法。
- 凍結体を水溶性有機溶媒に浸漬して水と有機溶媒の置換を行う操作を複数回繰り返すことにより、凍結体中の氷であった部分を有機溶媒に置換する、請求項1に記載のセラミック多孔体の製造方法。
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JP2007041513A JP5176198B2 (ja) | 2007-02-21 | 2007-02-21 | マクロポーラスな連通孔を持つセラミック多孔体の製造方法 |
PCT/JP2008/052846 WO2008102801A1 (ja) | 2007-02-21 | 2008-02-20 | マクロポーラスな連通孔を持つセラミック多孔体及びその製造方法 |
US12/527,924 US8262957B2 (en) | 2007-02-21 | 2008-02-20 | Ceramic porous body with communication macropores and process for producing the ceramic porous body |
EP08711652.1A EP2133317A4 (en) | 2007-02-21 | 2008-02-20 | POROUS CERAMIC BODY WITH COMMUNICATION MACROPORES AND METHOD FOR PRODUCING THE POROUS CERAMIC BODY |
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