TW201035000A - Process for producing a fired body of aluminum titanate-based ceramics and a fired body of aluminum titanate-based ceramics - Google Patents

Process for producing a fired body of aluminum titanate-based ceramics and a fired body of aluminum titanate-based ceramics Download PDF

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TW201035000A
TW201035000A TW98145228A TW98145228A TW201035000A TW 201035000 A TW201035000 A TW 201035000A TW 98145228 A TW98145228 A TW 98145228A TW 98145228 A TW98145228 A TW 98145228A TW 201035000 A TW201035000 A TW 201035000A
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aluminum titanate
powder
sintered body
based ceramic
weight
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TW98145228A
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Chinese (zh)
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Masayuki Narumi
Tetsuro Tohma
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Sumitomo Chemical Co
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    • 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
    • C04B35/462—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 based on titanates
    • C04B35/478—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 based on titanates based on aluminium titanates
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
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  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Filtering Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Processes For Solid Components From Exhaust (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)

Abstract

Disclosed is a method for producing an aluminum titanate ceramic sintered body, wherein the shrinkage of a green body during sintering is reduced. Also disclosed is an aluminum titanate ceramic sintered body having a low thermal expansion coefficient and a high porosity. In the method for producing an aluminum titanate ceramic sintered body, 2-25 parts by weight of an inorganic oxide powder is mixed per 100 parts by weight of an aluminum titanate ceramic powder, the thus-obtained mixture is formed into a green body, and the thus-obtained green body is sintered. The aluminum titanate ceramic sintered body is obtained by the method.

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201035000 六、發明說明： 【發明所屬之技術領域】 本發明係有關鈦酸鋁系陶瓷燒結體之製造方法及纟太酸 • 鋁系陶瓷燒結體。 【先前技術】 已知鈦酸鋁系陶瓷爲，含有構成元素之鈦及鋁，於X ^ 線衍射光譜中具有鈦酸鋁之結晶圖型的陶瓷中，具有優良 耐熱性之陶瓷。先前鈦酸鋁系陶瓷係作爲坩堝等燒結用器 具等用。又既使該類鈦酸鋁系陶瓷燒結體中之多孔質燒結 體，近年來係將其作爲構成捕集自柴油機等內燃機關排出 之排氣所含的微細碳粒子用之陶瓷濾器材料用，以提高產 業上利用價値。 捕集自柴油機排出之油烟等浮游微粒物質用的柴油微 粒子濾器（DPF) —般係自具有高氣孔率之蜂窩形狀的陶瓷 Q 燒結體形成。使用自該多孔質陶瓷形成之DPF時，需進行 於濾器上燃燒蜂窩壁上捕集的油烟以回復通氣阻力之再生 處理。此時DPF用蜂窩內溫度會急速上升，而使DPF用 _ 蜂窩暴露於高溫，同時接受極大的熱衝擊。又，以柴油機 ^ 作爲汽車或2程機具之動力源用時，使用中會曝露於極大 之機械震動中。因此對DPF之蜂窩所使用的陶瓷燒結體要 求具有較高耐熱衝擊性及機械強度，使來自熱疲勞之特性 惡化値較小。 已知該類鈦酸鋁系陶瓷燒結體之製造方法爲，將造孔 -5- 201035000 劑、黏合劑、水等加入欽酸銘系陶瓷粉末中，使所得混合 物成形後燒結之方法。 先前技術文獻 專利文獻 專利文獻1:特許第3185960號公報 【發明內容】 發明所欲解決之課題 但將鈦酸鋁系陶瓷粉末成形製作多孔質燒結體時，會 因鈦酸鋁系陶瓷粉末之保形性變差，而使燒結時增加收 縮’故燒結時易發生成形體崩塌及裂開。特別是現今針對 汽車及2程機具用途之柴油機加強其排氣規範下，一般要 求構成DPF用之多孔質蜂窩形狀爲大型的直徑1 OOmmx 長 100mm以上’其壁厚度薄化爲〇.5mm以下，單元構造具 有3 0 0小室以上，有效氣孔率爲3 0至6 0 v ο 1 %，平均細孔 直徑爲1至20μηι，細孔徑分布具有（D5〇-D10)/D50未達 0.5之狹窄細孔分布般非常脆弱構造。另外決定DPF之耐 熱衝擊性的重大要素中需倂有較低熱膨脹特性（熱膨脹率 較佳爲未達I.SxlO^K'1)及較高機械強度。因此製作DPF 用燒結體時，爲了確保成形性及燒結時之保形性以減少收 縮率，而寄望於開發具有較低熱膨脹係數之鈦酸鋁系陶瓷 燒結體及其製造方法。 有關確保保形性之方法，專利文獻1曾揭示具有雙樣 式粒度分布之駄酸銘粉末的製造方法，但該方法會增加燒 -6- 201035000 成時成形體之收縮率，降低所得燒結體之氣孔率而增加熱 膨脹率，因此尙不足以作爲D P F用鈦酸鋁系陶瓷燒結體之 製造方法用。 本發明之目的爲，提供可降低燒結時燒結體之收縮率 的鈦酸鋁系陶瓷燒結體之製造方法，及具有較低熱膨脹係 數與較高氣孔率之鈦酸鋁系陶瓷燒結體。 解決課題之方法 本發明之鈦酸鋁系陶瓷燒結體的製造方法爲，特徵係 相對於鈦酸鋁系陶瓷粉末1 〇 〇重量份混合2至2 5重量份 之無機氧化物粉末後，將所得混合物成形再燒結所得的成 形體。 前述無機氧化物爲氧化鋁。前述鈦酸鋁系陶瓷粉末之 平均粒徑較佳爲5至5 0 μπι。 又，無機氧化物粉末之平均粒徑較佳爲 0. I至 1 5 μηι。相對於無機氧化物粉末之平均粒徑的鈦酸鋁系陶瓷 粉末之平均粒徑的比較佳爲3以上，更佳爲5至5 0。 本發明之燒結溫度較佳爲1 3 00至1 6 5 0 °C。 又本發明係提供，相對於鈦酸鋁系陶瓷粉末1 〇〇重量 份混合2至2 5重量份之無機氧化物粉末後，使所得混合 物成形，再燒結所得的成形體而得之鈦酸鋁系陶瓷燒結 體。 前述鈦酸鋁系陶瓷燒結體較佳爲，氣孔率爲3 0至 60%之多孔質燒結體。 201035000 本發明也包含，自前述鈦酸鋁系陶瓷燒結體形成的柴 油微粒子濾器。 發明之效果 因本發明爲鈦酸鋁系陶瓷粉末混合特定範圍之含量的 無機氧化物粉末後，使所得混合物成形，再燒結所得的成 形體，故可降低燒結時成形體之收縮率，及使所得燒結體 實現較高氣孔率及較低的熱膨脹係數。又藉由調節無機氧 化物之混合物，可控制燒結時之鈦酸鋁系陶瓷成形體的收 縮率。 實施發明之形態 本發明之鈦酸鋁系陶瓷燒結體的製造方法爲，相對於 鈦酸鋁系陶瓷粉末1 〇〇重量份混合2至25重量份之無機 氧化物粉末後成形、燒結。因此可安定自先前於燒結中多 半會使成形體崩塌、成形體易發生龜裂或裂開，且成形體 出現較大燒結收縮之鈦酸鋁系陶瓷粉末，製作多孔質燒結 體。又該燒結時之鈦酸鋁系陶瓷成形體的燒結收縮率（線 收縮率）具體上可由，將鈦酸鋁系陶瓷粉末及無機氧化物 粉末之混合物壓縮成形爲一定形狀後測定成形體之邊長， 再測定該成形體燒結後之邊長而算出。 本發明可藉由鈦酸鋁系陶瓷粉末混合無機氧化物粉 末，再降低燒結時之鈦酸鋁系陶瓷成形體的收縮率，另可 藉由調整無機氧化物粉末混合量而控制前述收縮率。又無 -8- 201035000 機氧化物粉末具有提昇鈦酸鋁系陶瓷燒結體之機械強度的 效果。無機氧化物粉末之混合量相對於鈦酸鋁系陶瓷粉末 1 〇〇重量份爲未達2重量份時，將無法得到充分的前述收 縮率降低效果而不宜。又無機氧化物粉末之混合量相對於 ' 鈦酸鋁系陶瓷粉末1 〇〇重量份爲超過25重量份時，比較 未添加時會大幅增加熱膨脹係數，而減少氣孔率，另外會 因無機氧化物粉末之種類而提高成形體的收縮率故不宜。 ^ 無機氧化物粉末之混合量相對於鈦酸鋁系陶瓷粉末1 00重 量份更佳爲5至2 0重量份。 無機氧化物如，氧化鋁、二氧化鈦、氧化鎂、二氧化 矽、氧化鐵、模來石、謹青石等，此等無機氧化物可同時 使用二種以上。其中就固熔於鈦酸鋁系陶瓷中，與鈦酸鋁 系陶瓷反應時不會形成新的化合物，以及熔點高於鈦酸鋁 系陶瓷時爲難燒結性等理由，所使用的控制鈦酸鋁系陶瓷 之燒結收縮舉動的無機氧化物粉末較佳爲氧化鋁。本發明 Q 可適用的氧化鋁之結晶型如，T型、5型、Θ型、α型 等，又氧化鋁可爲非晶質。氧化鋁又以燒結時不會伴隨體 積收縮而出現結晶變態之α型的氧化鋁爲佳。 '本發明所使用的鈦酸鋁系陶瓷粉末之平均粒徑較佳爲 5至50μιη之範圍內，更佳爲10至30μηι之範圍內。鈦酸 鋁系陶瓷粉末之平均粒徑爲未達5μηι時，爲了得到所希望 之氣孔率及細孔徑傾向於需大量造孔劑，又超過5 0 μ m時 會明顯降低成形性而傾向於難得到所希望形狀之成形體。 此時之粉末的平均粒徑爲，利用雷射衍射測定之粒徑分布 -9- 201035000 中，粒子之累積體積相對於測定用全體積爲5 0%之粒徑 (D50)。 所使用的無機氧化物爲上述氧化鋁時，較佳爲使用平 均粒徑（D50)0.1至15μηι之範圍內的氧化鋁，更佳爲使用 平均粒徑0.3至ΙΟμηι之範圍內的氧化銘。又氧化銘以外 之無機氧化物粉末的平均粒徑（D50)較佳爲0」至15μιη。 無機氧化物粉末之平均粒徑爲未達0 ·1 μm時，由於就以占 據於平均粒徑5至50μιη之鈦酸鋁系陶瓷粉末的粒子間隙 而言，其之尺寸爲小，而減少燒結收縮降低效果’又既使 少量添加也會增加鈦酸鋁系陶瓷之熱膨脹率。另外無機氧 化物粉末之平均粒徑超過1 5 μηι時’無機氧化物粉末無法 進入鈦酸鋁系陶瓷之粒子間隙，因此傾向於難賦予降低成 形體之收縮率。該無機氧化物粉末之平均粒徑爲’利用雷 射衍射法測定的相當於體積基準之累積百分率50%的粒徑 (D 5 0)的値。 另外相對於無機氧化物粉末之平均粒徑的鈦酸鋁系陶 瓷粉末之平均粒徑的比（（鈦酸鋁系陶瓷粉末之平均粒 徑）/(無機氧化物粉末之平均粒徑））較佳爲3以上，又以5 至50爲佳，更佳爲5至20。上述平均粒徑之比爲上述範 圍時，無機氧化物粒子（例如氧化鋁粒子）可有效率佔有鈦 酸鋁系陶瓷粉末之粒子間隙。 又，相對於無機氧化物粉末之平均粒徑的鈦酸鋁系陶 瓷粉末之平均粒徑的比爲5至2 0之範圍內時’無機氧化 物粉末之混合量相對於鈦酸鋁系陶瓷粉末1 00重量份較佳 -10- 201035000 爲2至1 5重量份。 鈦酸鋁系陶瓷粉末之構成相可僅爲鈦酸鋁（Al2Ti〇5)。 爲了提升鈦酸鋁之耐熱安定性，及降低燒結溫度之目 的’可爲使鎂（Mg)或鐵（Fe)固熔於鈦酸鋁（Ai2Ti〇5)而得 ' 之固熔體，特佳爲另含有鎂源粉末。固熔鎂而得之鈦酸 銘如組成式：A12 (1 - *) M g x T i! + χ 〇 5所示時，上述組成式中X 較佳爲0.01至0.5之範圍內，更佳爲0.05至ο」之範圍 內。 ❹ 該類鈦酸鋁粉末及鈦酸鋁鎂粉末爲了提升其燒結體之 強度之目的’可含有1至10重量份％之範圍之“〇2成 份。s i Ο 2成份之具體例如，s i 0 2玻璃、鋁矽酸鹽、鹼性長 石或玻璃料等。Si 02成份較佳爲以非晶質狀態均勻分散於 鈦酸鋁結晶粒子之粒界。 將上述鈦酸鋁系陶瓷粉末混合無機氧化物粉末而得之 混合物成形而得成形體後，藉由燒結該成形體可得鈦酸鋁 Q 系陶瓷燒結體。成形後藉由燒結可抑制燒結中成形體收 縮，因此可抑制防止所得鈦酸鋁系陶瓷燒結體裂開。成形 體之形狀並無特別限制，例如可爲蜂窩形狀、棒狀、管 狀、板狀、坩堝形狀等。 成形用之成形機如，單軸加壓機、擠壓成形機、打錠 機、造粒機等。進行擠壓成形時，鈦酸鋁系陶瓷粉末及無 機氧化物粉末可添加例如造孔劑、黏合劑、潤滑劑、可塑 劑、分散劑、溶劑等添加劑而成形。 上述造孔劑如，石墨等碳材料；聚乙烯、聚丙烯、聚 -11 - 201035000 甲基丙稀酸甲酯等樹脂類；澱粉、花生殻、核桃殼、玉米 等植物系材料；冰及乾冰等。造孔劑之添加量相對於鈦酸 銘系陶瓷粉末及無機氧化物粉末之合計量100重量份，一 般爲0.5至40重量份，較佳爲1至25重量份。 上述黏合劑如，甲基纖維素、羧基甲基纖維素、鈉羧 基甲基纖維素等纖維素類；聚乙烯醇等醇類；木質系磺酸 鹽等鹽；石蠟、微晶蠟等蠟；EVA、聚乙烯、聚苯乙烯、 液晶聚合物、工程塑料等熱可塑性樹脂等。黏合劑之添加 量相對於鈦酸鋁系陶瓷粉末及無機氧化物粉末之合計量 1〇〇重量份，一般爲0.5至20重量份，較佳爲1至15重 量份。 上述潤滑劑及可塑劑如，甘油等醇類；癸酸、月桂 酸、棕櫚酸、花生酸、油酸、硬脂酸等高級脂肪類；硬脂 酸鋁等硬酯酸金屬鹽等。潤滑劑及可塑劑之添加量相對於 鈦酸鋁系陶瓷粉末及無機氧化物粉末之合計量100重量 份，一般爲〇至1〇重量份。 上述分散劑如，硝酸、鹽酸、硫酸等無機酸；草酸、 檸檬酸、乙酸、蘋果酸、乳酸等有機酸；甲醇 '乙醇、丙 醇等醇類；聚羧酸銨、聚氧化烯烴烷醚等表面活性劑等。 分散劑之添加量相對於鈦酸鋁系陶瓷粉末及無機氧化物粉 末之合計量100重量份’一般爲0至20重量份’較佳爲2 至8重量份。 又，上述溶劑可使用甲醇、乙醇、丁醇、丙醇等1價 醇類；丙二醇、聚丙二醇 '乙二醇等2價醇類；及水。其 -12- 201035000 中又以不純物較少之水爲佳，更佳爲使用離子交換水。溶 齊！ί β使用量相對於鈦酸鋁系陶瓷粉末及無機氧化物粉末之 合計量100重量份，一般爲10至100重量份，較佳爲20 至8 0重量份。 " 混合（混練）上述鈦酸鋁系陶瓷粉末、無機氧化物粉末 及上述各種添加劑後，將混合物供給例如擠壓成形等成 形’可得所希望之形狀的成形體。 0 燒結成形體之燒結溫度一般爲1 30(TC以上，較佳爲 1 400 °C以上。又燒結溫度一般爲1 650 °C以下，較佳爲 1 5 5〇°C以下。到達燒結溫度之升溫速度並無特別限定，一 般爲1 °C /小時至5〇(TC /小時。成形體含有黏合劑等添加燃 燒性有機物時，燒結過程中係包含去除其用之脫脂步驟。 典型的脫脂係於到達燒結溫度之升溫階段（例如！ 50至4〇〇 °C之溫度範圍）完成。脫脂步驟較佳爲極力抑制升溫速 度。 Q 燒結一般係於大氣中進行，又可於氮氣、氬氣等不活 性氣體中燒結’或可於一氧化碳氣體、氫氣等還原性氣體 中燒結。又可於降低水蒸氣分壓之環境中進行燒結。 一般燒結係使用管狀電爐、箱型電爐、隧道爐、遠紅 外線爐、微波加熱爐、軸爐、反射爐、回轉爐、輕室爐等 一般的燒結爐進行。燒結可以分批式，或連續式進行。又 可以靜置式進行，或以流動式進行。 燒結所需時間可爲，成形體能充分遷移至鈦酸鋁系燒 結體之時間，可依鈦酸鋁系陶瓷粉末、無機氧化物粉末等 -13- 201035000 之含量、燒結爐之形式、燒結溫度、燒結環境等而異，一 般爲1 0分鐘至2 4小時。 如上述可得目的之鈦酸鋁系陶瓷燒結體。該類鈦酸鋁 系陶瓷燒結體可具有幾乎維持成形後成形體之形狀的形 狀。所得的鈦酸鋁系陶瓷燒結體可利用硏硝加工等，加工 爲所希望之形狀。 本發明之鈦酸鋁系陶瓷燒結體較佳爲，氣孔率3 0至 6 0 %之多孔質燒結體，更佳爲氣孔率3 5至5 5 %，特佳爲氣 孔率37至50%，其適用爲柴油微粒子濾器。 【實施方式】 下面將舉實施例、比較例更詳細說明本發明，但本發 明非限於此等。 <實施例1 > 相對於平均粒徑（D 5 0)24μηι鈦酸鋁鎂粉末（Recotherm, OHCERA(股）製）1〇〇重量份，混合平均粒徑（〇50)2.3μιη之 氧化鋁粉末（AL-M41)，住友化學（股）製）5重量份。以組成 式：[Technical Field] [Invention] The present invention relates to a method for producing an aluminum titanate-based ceramic sintered body and a samarium acid-aluminum-based ceramic sintered body. [Prior Art] It is known that an aluminum titanate-based ceramic is a ceramic having excellent heat resistance in a ceramic having a crystal form of aluminum titanate in a X-ray diffraction spectrum, containing titanium and aluminum as constituent elements. The aluminum titanate-based ceramics are used as a sintering tool such as tantalum. In addition, in recent years, the porous sintered body of the aluminum titanate-based ceramics sintered body has been used as a ceramic filter material for fine carbon particles contained in exhaust gas discharged from an internal combustion engine such as a diesel engine. In order to increase the utilization price of the industry. A diesel particulate filter (DPF) for collecting suspended particulate matter such as soot discharged from a diesel engine is generally formed from a sintered ceramic Q sintered body having a high porosity. When the DPF formed of the porous ceramic is used, it is necessary to carry out the regeneration of the soot trapped on the honeycomb wall of the filter to restore the ventilation resistance. At this time, the temperature inside the DPF will rise rapidly, and the DPF will be exposed to high temperatures by the _cell while receiving a great thermal shock. In addition, when the diesel engine is used as the power source for the car or the 2-way machine, it will be exposed to great mechanical vibration during use. Therefore, the ceramic sintered body used for the honeycomb of the DPF is required to have high thermal shock resistance and mechanical strength, and the characteristics from thermal fatigue are deteriorated to a small extent. It is known that a method for producing such an aluminum titanate-based ceramic sintered body is a method in which a hole of -5 - 201035000, a binder, water, or the like is added to a ceramic powder of a cinnamic acid to form a mixture and then sintered. [Problem to be Solved by the Invention] However, when an aluminum titanate-based ceramic powder is molded into a porous sintered body, it is protected by an aluminum titanate-based ceramic powder. The shape is deteriorated, and the shrinkage is increased during sintering. Therefore, the formed body is liable to collapse and crack when sintered. In particular, today's diesel engines for automobiles and two-pass machines are reinforced with their exhaust specifications. Generally, the shape of the porous honeycomb used to form the DPF is large, and the diameter of the porous body is 100 mm or more and 100 mm or more. The wall thickness is reduced to less than 5 mm. The unit structure has more than 300 chambers, an effective porosity of 30 to 60 v ο 1 %, an average pore diameter of 1 to 20 μm, and a pore size distribution having a narrowness of (D5〇-D10)/D50 of less than 0.5. The pores are distributed as a very fragile structure. In addition, it is necessary to have a lower thermal expansion characteristic (the thermal expansion rate is preferably less than I.SxlO^K'1) and a high mechanical strength in determining the thermal shock resistance of the DPF. Therefore, in the production of a sintered body for DPF, in order to secure moldability and shape retention during sintering to reduce the shrinkage ratio, it is expected to develop a sintered aluminum titanate-based ceramic body having a low coefficient of thermal expansion and a method for producing the same. Regarding the method for ensuring the shape retention property, Patent Document 1 discloses a method for producing a tannic acid powder having a double-pattern particle size distribution, but this method increases the shrinkage ratio of the formed body at the time of firing -6-201035000, and lowers the obtained sintered body. Since the porosity is increased and the coefficient of thermal expansion is increased, it is not sufficient as a method for producing a sintered aluminum titanate-based ceramic body for DPF. An object of the present invention is to provide a method for producing an aluminum titanate-based ceramic sintered body which can reduce the shrinkage ratio of a sintered body during sintering, and an aluminum titanate-based ceramic sintered body having a low thermal expansion coefficient and a high porosity. Solution to Problem The method for producing an aluminum titanate-based ceramic sintered body of the present invention is characterized in that 2 to 25 parts by weight of the inorganic oxide powder is mixed with 1 part by weight of the aluminum titanate-based ceramic powder. The resulting mixture was shaped and then sintered. The aforementioned inorganic oxide is alumina. The aluminum titanate-based ceramic powder preferably has an average particle diameter of 5 to 50 μm. Further, the average particle diameter of the inorganic oxide powder is preferably from 0.1 to 15 μm. The average particle diameter of the aluminum titanate-based ceramic powder with respect to the average particle diameter of the inorganic oxide powder is preferably 3 or more, more preferably 5 to 50. The sintering temperature of the present invention is preferably from 1 3 00 to 1 60 50 °C. Further, the present invention provides an aluminum titanate obtained by mixing 2 to 25 parts by weight of the inorganic oxide powder with respect to 1 part by weight of the aluminum titanate-based ceramic powder, and then forming the obtained mixture and sintering the obtained shaped body. A ceramic sintered body. The aluminum titanate-based ceramic sintered body is preferably a porous sintered body having a porosity of 30 to 60%. 201035000 The present invention also encompasses a diesel particulate filter formed from the above-described aluminum titanate-based ceramic sintered body. According to the present invention, since the aluminum titanate-based ceramic powder is mixed with the inorganic oxide powder in a specific range, the obtained mixture is molded and the obtained molded body is sintered, so that the shrinkage ratio of the molded body at the time of sintering can be reduced and The resulting sintered body achieves a higher porosity and a lower coefficient of thermal expansion. Further, by adjusting the mixture of the inorganic oxides, the shrinkage ratio of the aluminum titanate-based ceramics formed during sintering can be controlled. EMBODIMENT OF THE INVENTION In the manufacturing method of the aluminum titanate-based ceramics sintered body of the present invention, 2 to 25 parts by weight of the inorganic oxide powder is mixed with 1 part by weight of the aluminum titanate-based ceramic powder, followed by molding and sintering. Therefore, it is possible to stabilize the aluminum titanate-based ceramic powder in which the molded body is collapsed, the molded body is likely to be cracked or cracked, and the molded body exhibits large sintering shrinkage, and a porous sintered body is produced. Further, the sintering shrinkage ratio (linear shrinkage ratio) of the aluminum titanate-based ceramics molded body at the time of sintering can be specifically determined by compressing and molding a mixture of an aluminum titanate-based ceramic powder and an inorganic oxide powder into a predetermined shape, and then measuring the side of the molded body. The length of the molded body after the sintering was measured was measured. In the present invention, the inorganic oxide powder is mixed with the aluminum titanate-based ceramic powder, and the shrinkage ratio of the aluminum titanate-based ceramic molded body at the time of sintering is reduced, and the shrinkage ratio can be controlled by adjusting the amount of the inorganic oxide powder. No -8- 201035000 The machine oxide powder has the effect of improving the mechanical strength of the aluminum titanate-based ceramic sintered body. When the amount of the inorganic oxide powder is less than 2 parts by weight based on 1 part by weight of the aluminum titanate-based ceramic powder, it is not preferable to obtain a sufficient effect of reducing the shrinkage ratio. When the amount of the inorganic oxide powder is more than 25 parts by weight based on 1 part by weight of the aluminum titanate-based ceramic powder, the coefficient of thermal expansion is greatly increased when the amount is not added, and the porosity is decreased, and the inorganic oxide is additionally caused. It is not preferable to increase the shrinkage rate of the molded body by the kind of the powder. The compounding amount of the inorganic oxide powder is more preferably 5 to 20 parts by weight based on 100 parts by weight of the aluminum titanate-based ceramic powder. Inorganic oxides such as alumina, titania, magnesia, cerium oxide, iron oxide, mullite, and cordierite may be used in combination of two or more kinds. Among them, the aluminum titanate ceramic is solid-melted, and a new compound is not formed when reacting with an aluminum titanate-based ceramic, and the aluminum silicate is used for the reason that the melting point is higher than that of the aluminum titanate-based ceramic. The inorganic oxide powder of the sintering shrinkage behavior of the ceramic is preferably alumina. The crystal form of alumina to which the present invention Q is applicable is, for example, T-type, 5-type, ruthenium-type, α-type, etc., and alumina may be amorphous. The alumina is preferably an α-type alumina which is crystallized and deformed without being accompanied by volume shrinkage during sintering. The average particle diameter of the aluminum titanate-based ceramic powder used in the present invention is preferably in the range of 5 to 50 μm, more preferably in the range of 10 to 30 μm. When the average particle diameter of the aluminum titanate-based ceramic powder is less than 5 μm, a large amount of pore-forming agent tends to be obtained in order to obtain a desired porosity and pore diameter, and when it exceeds 50 μm, the formability is remarkably lowered and it tends to be difficult. A shaped body of a desired shape is obtained. The average particle diameter of the powder at this time is a particle diameter distribution of -9 to 201035000 measured by laser diffraction, and the cumulative volume of the particles is 50% by particle diameter (D50) with respect to the entire volume for measurement. When the inorganic oxide to be used is the above alumina, it is preferred to use alumina having an average particle diameter (D50) of 0.1 to 15 μm, more preferably an oxide having a mean particle diameter of 0.3 to ΙΟμηι. Further, the average particle diameter (D50) of the inorganic oxide powder other than the oxide is preferably from 0" to 15 μm. When the average particle diameter of the inorganic oxide powder is less than 0.1 μm, since the particle gap of the aluminum titanate-based ceramic powder which occupies an average particle diameter of 5 to 50 μm is small, the sintering is reduced. The shrinkage reduction effect', even a small amount of addition, also increases the thermal expansion rate of the aluminum titanate-based ceramics. Further, when the average particle diameter of the inorganic oxide powder exceeds 15 μm, the inorganic oxide powder cannot enter the particle gap of the aluminum titanate-based ceramic, and thus it tends to be difficult to impart a reduction in the shrinkage ratio of the formed body. The average particle diameter of the inorganic oxide powder is 値 which is a particle diameter (D 5 0) corresponding to a cumulative percentage of a volume basis of 50% measured by a laser diffraction method. Further, the ratio of the average particle diameter of the aluminum titanate-based ceramic powder to the average particle diameter of the inorganic oxide powder ((the average particle diameter of the aluminum titanate-based ceramic powder) / (the average particle diameter of the inorganic oxide powder)) Preferably, it is 3 or more, and preferably 5 to 50, more preferably 5 to 20. When the ratio of the above average particle diameter is in the above range, the inorganic oxide particles (e.g., alumina particles) can efficiently occupy the particle gap of the aluminum titanate-based ceramic powder. Further, when the ratio of the average particle diameter of the aluminum titanate-based ceramic powder to the average particle diameter of the inorganic oxide powder is in the range of 5 to 20, the amount of the inorganic oxide powder is mixed with respect to the aluminum titanate-based ceramic powder. 100 parts by weight is preferably from -10-201035000 to 2 to 15 parts by weight. The constituent phase of the aluminum titanate-based ceramic powder may be only aluminum titanate (Al 2 Ti 〇 5). In order to improve the heat stability of aluminum titanate and reduce the sintering temperature, it is a solid solution for solid-melting magnesium (Mg) or iron (Fe) to aluminum titanate (Ai2Ti〇5). It is a powder containing magnesium source. The titanic acid obtained by solid-melting magnesium is as shown in the composition formula: A12 (1 - *) M gx T i! + χ 〇 5, wherein X is preferably in the range of 0.01 to 0.5, more preferably Within the range of 0.05 to ο". ❹ The aluminum titanate powder and the aluminum magnesium titanate powder may contain “〇2 component in the range of 1 to 10% by weight for the purpose of improving the strength of the sintered body. The specific composition of the Si Ο 2 component, for example, si 0 2 Glass, aluminosilicate, alkaline feldspar or glass frit, etc. The Si 02 component is preferably uniformly dispersed in the amorphous state in the grain boundary of the aluminum titanate crystal particles. The aluminum titanate-based ceramic powder is mixed with the inorganic oxide. After the obtained mixture of the powder is molded to obtain a molded body, the aluminum titanate Q-based ceramic sintered body can be obtained by sintering the formed body. The sintering of the formed body can be suppressed by sintering after the formation, thereby suppressing the prevention of the obtained aluminum titanate. The ceramic sintered body is cleaved. The shape of the molded body is not particularly limited, and may be, for example, a honeycomb shape, a rod shape, a tubular shape, a plate shape, a ruthenium shape, etc. A molding machine for molding such as a uniaxial pressing machine or extrusion molding Machine, ingot machine, granulator, etc. When extrusion molding, additives such as pore formers, binders, lubricants, plasticizers, dispersants, solvents, etc. may be added to the aluminum titanate-based ceramic powder and the inorganic oxide powder. Made The above pore-forming agent, such as carbon materials such as graphite; polyethylene, polypropylene, poly-11 - 201035000 methyl methacrylate and other resin; starch, peanut shell, walnut shell, corn and other plant materials; ice and Dry ice, etc. The amount of the pore former added is usually 0.5 to 40 parts by weight, preferably 1 to 25 parts by weight, based on 100 parts by weight of the total amount of the titanic acid ceramic powder and the inorganic oxide powder. , cellulose such as methyl cellulose, carboxymethyl cellulose, sodium carboxymethyl cellulose; alcohols such as polyvinyl alcohol; salts such as wood sulfonates; waxes such as paraffin wax and microcrystalline wax; EVA, polyethylene a thermoplastic resin such as polystyrene, a liquid crystal polymer, or an engineering plastic, etc. The amount of the binder added is generally 0.5 to 20 parts by weight based on 1 part by weight of the total amount of the aluminum titanate-based ceramic powder and the inorganic oxide powder. Parts, preferably 1 to 15 parts by weight. The above lubricants and plasticizers such as alcohols such as glycerin; higher fats such as capric acid, lauric acid, palmitic acid, arachidic acid, oleic acid, stearic acid; stearic acid Metal salts such as aluminum stearate, etc. Lubrication And the amount of the plasticizer added is generally from 1 to 10 parts by weight based on 100 parts by weight of the total amount of the aluminum titanate-based ceramic powder and the inorganic oxide powder. The above dispersing agent is an inorganic acid such as nitric acid, hydrochloric acid or sulfuric acid; , organic acids such as citric acid, acetic acid, malic acid, lactic acid; alcohols such as methanol 'ethanol and propanol; surfactants such as ammonium polycarboxylate and polyoxyalkylene alkyl ether. The amount of dispersant added is relative to aluminum titanate. The total amount of the ceramic powder and the inorganic oxide powder is 100 parts by weight 'generally 0 to 20 parts by weight', preferably 2 to 8 parts by weight. Further, the solvent may be monovalent using methanol, ethanol, butanol or propanol. Alcohols; divalent alcohols such as propylene glycol and polypropylene glycol 'ethylene glycol; and water. Among them, -12-201035000 is preferably water having less impurities, and more preferably ion-exchanged water. Dissolve! The amount of use of ί β is usually 10 to 100 parts by weight, preferably 20 to 80 parts by weight, based on 100 parts by weight of the total amount of the aluminum titanate-based ceramic powder and the inorganic oxide powder. " Mixing (kneading) the above aluminum titanate-based ceramic powder, inorganic oxide powder, and various additives described above, and then supplying the mixture to a molded article having a desired shape such as extrusion molding. 0 The sintering temperature of the sintered compact is generally 1 30 (TC or more, preferably 1 400 ° C or higher. The sintering temperature is generally 1 650 ° C or lower, preferably 15 5 ° ° C or lower. The heating rate is not particularly limited, and is generally from 1 ° C /hr to 5 Torr (TC / hr. When the molded body contains a binder, such as a binder, the degreasing step is removed during the sintering process. Typical degreasing system It is completed at the temperature rising stage of the sintering temperature (for example, the temperature range of 50 to 4 ° C). The degreasing step is preferably to suppress the heating rate as much as possible. Q Sintering is generally carried out in the atmosphere, and may be carried out in nitrogen or argon. Sintering in an inert gas' or sintering in a reducing gas such as carbon monoxide gas or hydrogen, and sintering in an environment where the partial pressure of water vapor is lowered. Generally, the sintering system uses a tubular electric furnace, a box type electric furnace, a tunnel furnace, and a far infrared ray. Furnace, microwave heating furnace, shaft furnace, reverberatory furnace, rotary furnace, light chamber furnace and other general sintering furnaces. Sintering can be carried out batchwise or continuously. It can be carried out in a static manner, or The time required for sintering may be the time during which the shaped body can fully migrate to the aluminum titanate-based sintered body, and may be in the form of a sintering furnace according to the content of the aluminum titanate-based ceramic powder, the inorganic oxide powder, and the like -13 - 201035000 In the sintering temperature, the sintering environment, and the like, it is generally from 10 minutes to 24 hours. The aluminum titanate-based ceramic sintered body can be obtained as described above. The aluminum titanate-based ceramic sintered body can be formed to almost form after molding. The shape of the shape of the body. The obtained aluminum titanate-based ceramic sintered body can be processed into a desired shape by a niobium nitrate processing or the like. The aluminum titanate-based ceramic sintered body of the present invention preferably has a porosity of 30 to 60. The porous sintered body of %, more preferably having a porosity of 35 to 5%, and particularly preferably having a porosity of 37 to 50%, is suitable for use as a diesel particulate filter. [Embodiment] Hereinafter, examples and comparative examples will be described in more detail. The present invention is described, but the present invention is not limited thereto. <Example 1 > With respect to the average particle diameter (D 5 0) 24 μηη aluminum magnesium titanate powder (Recotherm, manufactured by OHCERA), 1 part by weight, Mixed average particle size (〇50) 2.3μιη Alumina powder (AL-M41), 5 parts by weight of Sumitomo Chemical (shares), Ltd.) to form the formula:

Al2(1.x)MgxTi1+x〇5表示前述鈦酸鋁鎂粉末時之 X値爲 0.24，相對於該類鈦酸鋁鎂粉末及氧化鋁粉末之合計量 100重量份，加入造孔劑（FLO-THENE UF1 .5，住友精化 (股）製）15重量份及水3重量份後，進行30MPa、60秒之 單軸成形，再以1 4 5 0 °C燒結5小時，得鈦酸鋁鎂陶瓷燒結 -14- 201035000 體。 使用雷射粒度分析儀（sysmex股份公司製）測定粉末之 粒徑。又依據JIS R 1 634利用藉由水中浸漬之阿基米德 法，測定燒結體之水中重量M2(g)、飽水重量M3(g)及乾 ' 燥重量Ml(g)，再以下述式算出氣孔率。 氣孔率（％)=100χ(Μ3-Μ1)/(Μ3-Μ2) Θ 又，線收縮率係由測定鈦酸鋁系陶瓷粉末壓縮成形爲 某種形狀後之成形體邊長，及燒結該成形體後之邊長而算 出。 鈦酸鋁鎂陶瓷燒結體之熱膨脹率（ΚΓ1)爲，由各實施例 及各比較例所得的鈦酸鋁系陶瓷燒結體切出約4mm X約 4mm X約10mm之試驗片後，使用熱機械式分析裝置 (TMA6 3 00 - SIINanotechology(股）製）測定以 6〇〇°C/h 之升 Q 溫速度由室溫升至1 〇〇〇°C時上述角柱試料之熱膨脹曲線， 再算出室溫至1 〇〇〇°c間之溫度領域中的膨脹率而得。 <實施例2> 除了相對於鈦酸鋁鎂粉末1 0 0重量份混合氧化鋁粉末 1 〇重量份外，同實施例1得鈦酸鋁鎂陶瓷燒結體。 <實施例3 > 除了相對於鈦酸鋁鎂粉末1 00重量份混合氧化鋁粉末 -15- 201035000 用之平均粒徑（D50)6.6pin的氧化鋁粉末（AM-29B，住友化 學（股）製）5重量份外’同實施例1得鈦酸鋁鎂陶瓷燒結 體。 <實施例4> 除了相d於欽酸銘錶粉末1 0 0重量份混合氧化銘粉末 用之平均粒徑（D50)爲Ο.ΟΙμπι的氧化鋁粉末（AluC，日本 AEROSIL(股）製）5重量份外’同實施例1得鈦酸鋁鎂陶瓷 燒結體。 <實施例5 > 除了相對於鈦酸鋁鎂粉末1 00重量份混合氧化鋁粉末 用之平均粒徑（D50)l 6μιη的氧化鋁粉末（AT-50，住友化學 (股）製）5重量份外，同實施例1得鈦酸鋁鎂陶瓷燒結體。 <比較例1 > 除了未混合氧化鋁粉末外，同實施例1得鈦酸鋁鎂陶 瓷燒結體。 實施例1至5、比較例1之結果如表1所示。 -16- 201035000 [表i] 氧化鋁粉末之 氣孔率 收縮率 熱膨脹率 混合量(重量份) (%) (%) αο^κ·1) 實施例1 5 41.4 9.4 2.1 實施例2 10 41.6 9.0 2.2 實施例3 5 41.6 9.4 2.0 實施例4 5 44.3 9.9 2.4 實施例5 5 41.9 9.5 2.8 比較例1 0 40.5 10.2 2.3 <實施例6> 相對於平均粒徑（〇50)24μτη之鈦酸鋁鎂粉末 (Recotherm，OHCERA(股）製）1〇〇重量份，混合平均粒徑 (ϋ50)2·3μιη 之氧化鋁粉末（AL-M41，住友化學（股）製）5 重量份。以組成式：+ 表示前述鈦酸鋁 鎂粉末時之X値爲0.24。相對於該類鈦酸鋁鎂粉末及氧化 鋁粉末之合計量1 〇〇重量份，加入造孔劑用之聚乙烯粒子 (D5 0 = 2.3pm)10重量份、黏合劑用之甲基纖維素7.5重量 份、表面活性劑用之聚氧化烯烴烷醚9 · 3重量份、潤滑劑 用之甘油〇 · 8重量份而得成形原料後，加入分散劑用之水 3 8重量份，再使用混練機調製坯土，其後將坯土擠壓成形 製作蜂窩成形體。使用乾燥機以100°C乾燥蜂窩成形體12 小時後，大氣環境下使用箱型電爐以4〇〇°c實施去除黏合 劑用之脫脂步驟後，以3 00°C /h之速度升溫至I 45 0t，再 以1 45 0 °C燒結5小時’得鈦酸鋁鎂陶瓷之蜂窩燒結體。 <實施例7> -17- 201035000 除了相對於鈦酸鋁鎂粉末1 ο 〇重量份混合氧化鋁粉末 1 〇重量份外’同實施例6得鈦酸鋁鎂陶瓷之蜂窩燒結體。 <實施例8> 除了相對於鈦酸鋁鎂粉末1 00重量份混合氧化鋁粉末 用之平均粒徑（〇5〇)0·4μηι的氧化鋁粉末（AES_U，住友化 學（股）製）1〇重量份外，同實施例6得鈦酸鋁鎂陶瓷之蜂 窩燒結體。 <實施例9> 除了相對於鈦酸鋁鎂粉末1 0 0重量份混合氧化鋁粉末 用之平均粒徑（D50)0.4pm的氧化鋁粉末（AES-11，住友化 學（股）製）2 0重量份外，同實施例6得鈦酸鋁鎂陶瓷之蜂 窩燒結體。 <比較例2> 除了未混合氧化鋁粉末外，同實施例6得鈦酸鋁鎂陶 瓷之蜂窩燒結體。 <比較例3 > 除了相對於鈦酸鋁鎂粉末1 〇〇重量份混合氧化鋁粉末 用之平均粒徑（D50)0.4pm的氧化鋁粉末（AES-11，住友化 學（股）製）3 0重量份外，同實施例6得鈦酸鋁鎂陶瓷之蜂 窩燒結體。 -18 - 201035000 Ο 所得的實施例6至9、比較例2及3之蜂窩燒結體的 評估結果如表2所示。評估壓壞強度時，除了將上述坯土 擠壓成形爲直徑5mm、內徑2mm之管狀外，同蜂窩成形 體之條件製作燒結體，再以下述步驟進行。將管狀燒結體 備置於具備自在移動之移動壓具的加壓驅動裝置，藉由使 前述壓具朝向下方向以一定速度降下，對管狀燒結體朝向 下方向施加以一定速度增加之荷重，藉由測力傳感器測定 管狀燒結體之擠壓方向的壓壞強度。 表2 氧化鋁粉末之 混合量(重量份） 氣孔率 (%) 收縮率 (%) 熱膨脹率 (ΙΟ^Κ·1) 壓壞強度 (MPa) 實施例6 5 41.5 8.8 1.7 21.8 實施例7 10 40.4 8.3 1.5 26.4 實施例8 10 39.1 10.2 1.3 25.7 實施例9 20 37.2 10.1 1.8 32.9 比較例2 0 41.6 11.4 1.9 18.0 比較例3 30 34.5 10.1 2.1 44.9 〇 比較未添加氧化鋁粉末之比較例2，添加2 5重量份以 下之氧化鋁粒子的實施例6至9之蜂窩燒結體的氣孔率幾 乎一定，且收縮率較低爲1至3 %，熱膨脹率較小可提升 機械強度。又添加過剩的3 0重量份之氧化銘粒子的比較 例3之蜂窩燒結體，比較未添加氧化鋁粉末之比較例2 時，其氣孔率會降低5 %以上’且來自氧化鋁原有較大的 熱膨脹率，會傾向使蜂窩燒結體之熱膨脹率較大。 此次揭示之實施形態及實施例均爲例示並無限制。本 -19- 201035000 發明之範圍除了上述所說明可依申請專利範圍所表示包 含，均等於專利範圍之內容、及範圍內所有變更情形。 產業上利用可能性 本發明所得的鈦酸鋁系陶瓷燒結體適用於’例如坩 堝、調節器、乳鉢、爐材等燒結爐用器具；柴油機、汽油 機等內燃機關之排氣氣體淨化用的排氣濾器，及觸媒載 體、啤酒等飲食過濾用之濾器，精製石油時選擇性使所生 成之氣體成份，例如一氧化碳、二氧化碳、氮、氧等透過 用的選擇透過濾器等陶瓷濾器；基板、電容器等電子構件 等。其中使用於陶瓷濾器等時’本發明之鈦酸鋁系陶瓷燒 結體因具有比先前更大之氣孔率，故可具有優良濾器性能 (排氣處理能力、堆高能力、壓力損失等）。 -20-Al2(1.x)MgxTi1+x〇5 indicates that the X値 of the aluminum magnesium titanate powder is 0.24, and a pore former is added to 100 parts by weight of the total amount of the aluminum magnesium titanate powder and the aluminum oxide powder. FLO-THENE UF1.5, Sumitomo Seika Co., Ltd.) 15 parts by weight and 3 parts by weight of water, uniaxially formed at 30 MPa and 60 seconds, and sintered at 1 450 ° C for 5 hours to obtain titanic acid. Aluminum-magnesium ceramic sintered -14- 201035000 body. The particle size of the powder was measured using a laser particle size analyzer (manufactured by sysmex AG). Further, according to JIS R 1 634, the weight of the sintered body M2 (g), the weight of the saturated water M3 (g), and the dry weight Ml (g) were measured by the Archimedes method impregnated with water, and then the following formula was used. Calculate the porosity. Porosity (%)=100χ(Μ3-Μ1)/(Μ3-Μ2) Θ Further, the linear shrinkage ratio is obtained by measuring the side length of the molded body after compression molding of the aluminum titanate-based ceramic powder into a certain shape, and sintering. Calculated by the length of the side of the body. The thermal expansion coefficient (ΚΓ1) of the aluminum titanate-calcium ceramic sintered body is obtained by cutting a test piece of about 4 mm X, about 4 mm X, and about 10 mm from the aluminum titanate-based ceramic sintered body obtained in each of the examples and the comparative examples, and then using a thermomechanical machine. Analytical apparatus (TMA6 3 00 - manufactured by SIINanotechology Co., Ltd.) measures the thermal expansion curve of the above-mentioned prism sample at room temperature of 6 ° C / h from room temperature to 1 ° ° C, and then calculates the chamber It is obtained by the expansion rate in the temperature range between 1 〇〇〇 ° °C. <Example 2> An aluminum titanate magnesium ceramic sintered body was obtained in the same manner as in Example 1 except that 100 parts by weight of the alumina powder was mixed with 1 part by weight of the aluminum magnesium titanate powder. <Example 3 > In addition to 100 parts by weight of alumina powder mixed with aluminum magnesium titanate powder -15-201035000, an average particle diameter (D50) of 6.6 pin of alumina powder (AM-29B, Sumitomo Chemical Co., Ltd. And 5 parts by weight of the same as in Example 1 obtained as an aluminum titanate magnesium ceramic sintered body. <Example 4> Alumina powder having an average particle diameter (D50) of 混合.ΟΙμπι (AluC, manufactured by Japan AEROSIL Co., Ltd.) was used in addition to the phase d of the acid powder 5 parts by weight of the same as in Example 1 obtained an aluminum titanate magnesium ceramic sintered body. <Example 5> Alumina powder (AT-50, manufactured by Sumitomo Chemical Co., Ltd.) 5 having an average particle diameter (D50) of 6 μιη mixed with alumina powder for 100 parts by weight of aluminum magnesium titanate powder A sintered body of an aluminum titanate ceramic of the same manner as in Example 1 was obtained. <Comparative Example 1 > An aluminum titanate ceramic sintered body was obtained in the same manner as in Example 1 except that the alumina powder was not mixed. The results of Examples 1 to 5 and Comparative Example 1 are shown in Table 1. -16- 201035000 [Table i] Porosity shrinkage rate of alumina powder Coefficient of thermal expansion (parts by weight) (%) (%) αο^κ·1) Example 1 5 41.4 9.4 2.1 Example 2 10 41.6 9.0 2.2 Example 3 5 41.6 9.4 2.0 Example 4 5 44.3 9.9 2.4 Example 5 5 41.9 9.5 2.8 Comparative Example 1 0 40.5 10.2 2.3 <Example 6> Aluminum magnesium titanate powder with an average particle diameter (〇50) of 24 μτη (Recotherm, manufactured by OHCERA Co., Ltd.) 5 parts by weight of alumina powder (AL-M41, manufactured by Sumitomo Chemical Co., Ltd.) having an average particle diameter (ϋ50) of 2·3 μm. The X 値 when the composition formula: + represents the aforementioned magnesium aluminum titanate powder is 0.24. 10 parts by weight of polyethylene particles (D5 0 = 2.3 pm) for the pore former, and methyl cellulose for the binder, based on 1 part by weight of the total amount of the aluminum magnesium titanate powder and the alumina powder. 7.5 parts by weight, 9.3 parts by weight of a polyoxyalkylene alkyl ether for a surfactant, and 8 parts by weight of a glycerin oxime for a lubricant, and then adding 38 parts by weight of water for a dispersing agent, and then kneading The clay was prepared by a machine, and then the clay was extruded to form a honeycomb formed body. After drying the honeycomb formed body at 100 ° C for 12 hours using a dryer, the degreasing step for removing the binder was carried out at 4 ° C using a box type electric furnace in an air atmosphere, and then the temperature was raised to 300 ° C / h at a rate of 300 ° C / h. 45 0t, and then sintered at 1 45 0 °C for 5 hours to obtain a honeycomb sintered body of aluminum magnesium titanate ceramic. <Example 7> -17- 201035000 A honeycomb sintered body of the aluminum titanate ceramics obtained in the same manner as in Example 6 except that the alumina powder was mixed with 1 part by weight of the aluminum magnesium titanate powder. <Example 8> Alumina powder (AES_U, manufactured by Sumitomo Chemical Co., Ltd.) having an average particle diameter (〇5〇) of 0·4 μηι used for mixing alumina powder with respect to 100 parts by weight of aluminum magnesium titanate powder A honeycomb sintered body of an aluminum titanate ceramic of the same manner as in Example 6 was obtained. <Example 9> Alumina powder (AES-11, manufactured by Sumitomo Chemical Co., Ltd.) 2 having an average particle diameter (D50) of 0.4 pm for mixing alumina powder with respect to 100 parts by weight of aluminum magnesium titanate powder In the same manner as in Example 0, a honeycomb sintered body of aluminum magnesium titanate ceramics was obtained in the same manner as in Example 6. <Comparative Example 2> A honeycomb sintered body of aluminum magnesium titanate ceramics was obtained in the same manner as in Example 6 except that the alumina powder was not mixed. <Comparative Example 3 > Alumina powder (AES-11, manufactured by Sumitomo Chemical Co., Ltd.) having an average particle diameter (D50) of 0.4 pm for mixing alumina powder with respect to 1 part by weight of aluminum magnesium titanate powder A honeycomb sintered body of an aluminum titanate ceramic of the same manner as in Example 6 was obtained, except for 30 parts by weight. -18 - 201035000 评估 The evaluation results of the obtained honeycomb sintered bodies of Examples 6 to 9 and Comparative Examples 2 and 3 are shown in Table 2. When the crush strength was evaluated, the sintered body was produced under the conditions of the honeycomb formed body except that the above-mentioned clay was extruded into a tubular shape having a diameter of 5 mm and an inner diameter of 2 mm, and the following steps were carried out. The tubular sintered body is placed in a pressurizing driving device having a moving presser that is free to move, and the presser is lowered at a constant speed in the downward direction, and the tubular sintered body is applied with a load increased at a constant speed in the downward direction. The load cell measures the crushing strength of the tubular sintered body in the extrusion direction. Table 2 Amount of alumina powder (parts by weight) Porosity (%) Shrinkage (%) Thermal expansion (ΙΟ^Κ·1) Crush strength (MPa) Example 6 5 41.5 8.8 1.7 21.8 Example 7 10 40.4 8.3 1.5 26.4 Example 8 10 39.1 10.2 1.3 25.7 Example 9 20 37.2 10.1 1.8 32.9 Comparative Example 2 0 41.6 11.4 1.9 18.0 Comparative Example 3 30 34.5 10.1 2.1 44.9 〇Comparative Example 2 without adding alumina powder, add 2 5 The honeycomb sintered bodies of Examples 6 to 9 of the parts by weight or less of alumina particles have almost a certain porosity and a low shrinkage ratio of 1 to 3%, and a small coefficient of thermal expansion can improve mechanical strength. Further, when the honeycomb sintered body of Comparative Example 3 in which 30 parts by weight of the oxidized particles were added, the porosity of the comparative example 2 in which the alumina powder was not added was decreased by 5% or more, and the original alumina was larger. The coefficient of thermal expansion tends to cause a large thermal expansion rate of the honeycomb sintered body. The embodiments and examples disclosed herein are illustrative and not limiting. The scope of the invention is intended to be inclusive of the scope of the patent and the scope of the invention. INDUSTRIAL APPLICABILITY The aluminum titanate-based ceramic sintered body obtained by the present invention is suitable for use in an apparatus for sintering furnaces such as crucibles, regulators, mortars, and furnace materials, and exhaust gas for exhaust gas purification such as diesel engines and gasoline engines. a filter, a filter for food filtration such as a catalyst carrier or a beer, and a ceramic filter such as a selective permeation filter for selectively permeable gas components such as carbon monoxide, carbon dioxide, nitrogen, and oxygen; and a substrate, a capacitor, etc. Electronic components, etc. When used in a ceramic filter or the like, the aluminum titanate-based ceramic sintered body of the present invention has excellent filter performance (exhaust gas treatment capacity, stacking capacity, pressure loss, etc.) because it has a larger porosity than before. -20-

Claims (1)

201035000 七、申請專利範圍： 1. 一種鈦酸鋁系陶瓷燒結體之製造 於鈦酸鋁系陶瓷粉末1 〇 〇重量份混合2 機氧化物粉末，使所得混合物成形後 脑 體。 2. 如申請專利範圍第1項之方法， 氧化鋁。 3. 如申請專利範圍第i或2項之方 陶瓷粉末之平均粒徑爲5至50μηι。 4 ·如申請專利範圍第1項之方法， 末之平均粒徑爲0.1至15μηι。 5 .如申請專利範圍第1項之方法， 粉末之平均粒徑相對於無機氧化物粉末 3以上。 6.如申請專利範圍第1項之方法 1300 至 1650。。。 7 · —種鈦酸鋁系陶瓷燒結體，其爲 陶瓷粉末100重量份混合2至25重量 末，使所得混合物成形後，燒結所得的; 8 ·如申請專利範圍第7項之鈦酸鋁 爲氣孔率30至60%之多孔質燒結體。 9. 一種柴油微粒子濾器，其爲，由 7或8項之鈦酸鋁系陶瓷燒結體形成。 方法，其爲，相對 至25重量份之無 ’燒結所得的成形 其中無機氧化物爲 法，其中鈦酸鋁系 其中無機氧化物粉 其中鈦酸鋁系陶瓷 之平均粒徑的比爲 ，其中燒結溫度爲 ，相對於鈦酸鋁系 份之無機氧化物粉 成形體而得。 系陶瓷燒結體，其 如申請專利範圍第 -21 - 201035000 四、指定代表圖：(一） 本案指定代表圖為：無 (二） 本代表圖之元件符號簡單說明：無201035000 VII. Scope of application: 1. Manufacture of an aluminum titanate-based ceramic sintered body. The aluminum titanate-based ceramic powder is mixed with 2 parts of oxide powder to make the resulting mixture into a body. 2. A method of applying for the patent scope, item 1, alumina. 3. The ceramic powder has an average particle size of 5 to 50 μm as in the scope of i or 2 of the patent application. 4 · As in the method of claim 1, the average particle size at the end is 0.1 to 15 μm. 5. The method of claim 1, wherein the powder has an average particle diameter of 3 or more with respect to the inorganic oxide powder. 6. The method of claim 1 1300 to 1650. . . 7 - an aluminum titanate-based ceramic sintered body which is obtained by mixing 2 to 25 parts by weight of a ceramic powder, and forming the obtained mixture, and then sintering the obtained mixture; 8 · The aluminum titanate according to item 7 of the patent application is A porous sintered body having a porosity of 30 to 60%. A diesel particulate filter which is formed of a sintered body of an aluminum titanate-based ceramic of 7 or 8. The method is that the ratio of the average particle diameter of the inorganic oxide powder to the aluminum titanate-based ceramic is as follows, wherein the ratio of the average particle diameter of the inorganic oxide powder to the aluminum oxide-based ceramic is The temperature is obtained from the inorganic oxide powder molded body of the aluminum titanate portion. Ceramic sintered body, as in the scope of patent application No. -21 - 201035000 IV. Designated representative map: (1) The representative representative of the case is: None (2) The symbol of the representative figure is simple: None -3- 201035000 五、本案若有化學式時，請揭示最能顯示發明特徵的化學 式：無-3- 201035000 5. If there is a chemical formula in this case, please reveal the chemical formula that best shows the characteristics of the invention: none
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