JPWO2013146953A1 - 多孔質材料、ハニカム構造体及び多孔質材料の製造方法 - Google Patents
多孔質材料、ハニカム構造体及び多孔質材料の製造方法 Download PDFInfo
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Abstract
Description
本発明の多孔質材料の一の実施形態は、図1に示されるように、骨材1と、「結合材3であるコージェライト中に強化粒子2であるムライト粒子が分散されたものであり細孔4を形成した状態で上記骨材1同士を結合する複合結合材5」と、を含有するものである。そして、本実施形態の多孔質材料は、金属珪素の含有量が15質量%未満である。また、金属珪素の含有量は、ICP(Inductively Coupled Plasma)−AES(発光分光分析)法で測定したSi、C、OからSiCとSiO2量を同定し、残りのSi量の値である。図1は、本発明の多孔質材料の一の実施形態(多孔質材料100)の断面を拡大して示す模式図である。
本発明のハニカム構造体は、上述した本発明の多孔質材料により構成され、「一方の端面から他方の端面まで延びる複数のセル」を区画形成する隔壁、を備えたものである。上記セルは、流体の流路となるものである。また、ハニカム構造体は、最外周に位置する外周壁を有する構造であることが好ましい。隔壁の厚さの下限値は、30μmが好ましく、50μmが更に好ましい。隔壁の厚さの上限値は、1000μmが好ましく、500μmが更に好ましく、350μmが特に好ましい。セル密度の下限値は、10セル/cm2が好ましく、20セル/cm2が更に好ましく、50セル/cm2が特に好ましい。セル密度の上限値は、200セル/cm2が好ましく、150セル/cm2が更に好ましい。
本発明の多孔質材料の製造方法について、以下に説明する。以下に説明する多孔質材料の製造方法は、多孔質材料によって構成される「ハニカム構造体」を、製造する方法でもある。
炭化珪素(SiC)粉末と複合結合材生成用原料粉末とを、7:3(体積比)の比率で混合して「混合粉末」を作製した。複合結合材生成用原料粉末としては、水酸化アルミニウムを45.1質量%、タルクを32.8質量%、シリカを22.1質量%含有する粉末を用いた。複合結合材生成用原料(粉末)中の酸化アルミニウム成分の含有率は、35.6質量%であった。また、複合結合材生成用原料(粉末)中の二酸化珪素成分の含有率は、51.8質量%であった。また、複合結合材生成用原料(粉末)中の酸化マグネシウム成分の含有率は、12.6質量%であった。そして、上記「混合粉末」に、バインダとしてヒドロキシプロピルメチルセルロース、造孔材としてデンプン、吸水性樹脂を添加すると共に、水を添加して成形原料とした。バインダの含有量は混合粉末を100質量部としたときに、7質量部であった。造孔材の含有量は混合粉末を100質量部としたときに、12質量部であった。水の含有量は混合粉末を100質量部としたときに、70質量部であった。炭化珪素粉末の平均粒子径は22.0μmであった。また、造孔材の平均粒子径は、20μmであった。なお、炭化珪素粉末及び造孔材の平均粒子径は、レーザー回折法で測定した値である。
多孔質材料(ハニカム構造体)における、各構成結晶相(複合結合材、ムライト粒子、金属珪素)の質量比率は以下のようにして求める。X線回折装置を用いて多孔質材料のX線回折パターンを得る。X線回折装置としては、回転対陰極型X線回折装置(理学電機製、RINT)を用いる。X線回折測定の条件は、CuKα線源、50kV、300mA、2θ=10〜60°とする。そして、「RIR(Reference Intensity Ratio)法を用いて、得られたX線回折データを解析して、各成分を定量する」簡易定量分析により、各構成結晶相の質量比率を算出する。X線回折データの解析は、MDI社製の「X線データ解析ソフトJADE7」を用いて行った。
ムライト粒子のアスペクト比(ムライトのアスペクト比)は、SEM(走査型電子顕微鏡)を用いて測定する。具体的には、3000倍の倍率で観察し得た微構造写真中の全てのムライト粒子の長径と短径を測定し、その比率「長径/短径」を算出し、微構造写真中のムライト粒子の個数で平均した値を、ムライトのアスペクト比とする。
ムライト粒子の長径は、SEM(走査型電子顕微鏡)を用いて測定する。具体的には、3000倍の倍率で観察し得た微構造写真中の全てのムライト粒子の長径を測定し、微構造写真中のムライト粒子の個数で平均した値を、ムライトの長径とする。
気孔率は、水銀圧入法(JIS R 1655準拠)による全細孔容積[cm3/g]と、アルキメデス法により測定した見掛密度[g/cm3]から算出する。気孔率の算出に際しては、「開気孔率(%)=100×全細孔容積/{(1/見掛密度)+全細孔容積}」の式を用いる。「全細孔容積」の測定(水銀圧入法)には、ハニカム構造体から「縦3セル×横3セル×長さ20mm」の大きさに切り出した試験片を用いる。また、見掛密度の測定(アルキメデス法)には、「20mm×20mm×0.3mm」の大きさ(20mm×20mmの大きさの1枚の隔壁に相当)に切り出した試験片を用いる。
ハニカム構造体から、「縦3セル×横3セル×長さ20mm」の大きさの試験片を切り出し、水銀圧入法(JIS R 1655準拠)により測定する。
「10μm以下の細孔容積率」及び「40μm以上の細孔容積率」は、以下のようにして測定する。上記「平均細孔径」の場合と同様の試験片を用いて、水銀圧入法(JIS R 1655準拠)により全細孔容積、細孔径が40μm以上である細孔の細孔容積、細孔径が10μm以下である細孔の細孔容積を測定する。そして、「10μm以下の細孔容積率」は10μm以下の細孔容積/全細孔容積、「40μm以上の細孔容積率」は40μm以上の細孔容積/全細孔容積の式で算出する。
ハニカム構造体をセルが貫通する方向を長手方向とした試験片(縦0.3mm×横4mm×長さ40mm)に加工し、JIS R1601に準拠した曲げ試験により曲げ強度を算出する。
上記「曲げ強度」の測定方法により「応力−歪曲線」を作成し、当該「応力−歪曲線」の傾きを算出する。得られた「応力−歪曲線の傾き」をヤング率とする。
JIS R1618に準拠する方法で、ハニカム構造体から縦3セル×横3セル×長さ20mmの試験片を切り出し、40〜800℃のA軸方向(ハニカム構造体の流路に対して平行方向)の平均線熱膨張係数(熱膨張係数)を測定する。
ハニカム構造体から、直径0.5mm×厚さ1.0mmの円盤状の測定試料を切り出す。得られた測定試料を用いてJIS R1611に準拠する方法で、室温における比熱を測定する。更に、測定試料について、アルキメデス法で、見かけ密度を測定する。そして、得られた比熱の値と見かけ密度との積を比熱容量(J/(cm3・K))とする。
各条件を表1〜8に示すものとした以外は実施例1と同様にして多孔質材料(ハニカム構造体)を作製した。実施例1の場合と同様にして、各評価を行った。結果を表1〜7に示す。また、複合結合材生成用原料中の酸化アルミニウム成分、酸化珪素成分及び酸化マグネシウム成分の含有率を表8に示した。尚、複合結合材生成用原料中の酸化アルミニウム成分、酸化珪素成分及び酸化マグネシウム成分の含有率は、使用した各原料の化学組成及び含有率から算出した。
Claims (15)
- 骨材と、結合材であるコージェライト中に強化粒子であるムライト粒子が分散されたものであり細孔を形成した状態で前記骨材同士を結合する複合結合材と、を含有し、
金属珪素の含有量が15質量%未満である多孔質材料。 - 前記骨材、前記複合結合材及び前記金属珪素の合計質量に対する、前記複合結合材の含有量の下限値が12質量%であり、前記複合結合材の含有量の上限値が50質量%である請求項1に記載の多孔質材料。
- 前記骨材、前記複合結合材及び前記金属珪素の合計質量に対する、前記ムライト粒子の含有量の下限値が0.5質量%であり、前記ムライト粒子の含有量の上限値が15質量%である請求項1又は2に記載の多孔質材料。
- 強化粒子である前記ムライト粒子の長径の下限値が0.5μmであり、前記ムライト粒子の長径の上限値が35μmである請求項1〜3のいずれかに記載の多孔質材料。
- 強化粒子である前記ムライト粒子のアスペクト比の下限値が1.5であり、前記ムライト粒子のアスペクト比の上限値が4.7である請求項1〜4のいずれかに記載の多孔質材料。
- 前記骨材が、炭化珪素(SiC)粒子及び窒化珪素(Si3N4)粒子の中の少なくとも一方を含有するものである請求項1〜5のいずれかに記載の多孔質材料。
- 気孔率の下限値が40%であり、気孔率の上限値が90%である請求項1〜6のいずれかに記載の多孔質材料。
- 細孔径10μm未満の細孔が細孔全体の20%以下であり、細孔径40μmを超える細孔が細孔全体の10%以下である請求項1〜7のいずれかに記載の多孔質材料。
- 曲げ強度が6.5MPa以上であり、曲げ強度/ヤング率比が1.4×10−3以上である請求項1〜8のいずれかに記載の多孔質材料。
- 熱膨張係数が4.2×10−6/K以下である請求項1〜9のいずれかに記載の多孔質材料。
- 請求項1〜10のいずれかに記載の多孔質材料により構成され、
一方の端面から他方の端面まで延びる複数のセルを区画形成する、隔壁を備えたハニカム構造体。 - 前記一方の端面における所定の前記セルの開口部及び前記他方の端面における残余の前記セルの開口部、に配設された目封止部を備える請求項11に記載のハニカム構造体。
- 骨材原料、複合結合材生成用原料、造孔材及びバインダを含有する成形原料を押出成形して成形体を作製する成形工程と、
前記成形体を不活性雰囲気にて1400〜1500℃で焼成して多孔質材料を作製する焼成工程とを有し、
前記複合結合材生成用原料が、34.9質量%超、71.8質量%未満の酸化アルミニウム成分、28.2質量%超、52.0質量%未満の二酸化珪素成分、及び5.0質量%超、13.8質量%未満の酸化マグネシウム成分を含有し、
前記多孔質材料中の金属珪素含有量が15質量%未満であり、
前記複合結合材生成用原料中に、金属珪素が含有されないか、又は得られる前記多孔質材料中の金属珪素含有量が15質量%未満となるような量の金属珪素が含有される、多孔質材料の製造方法。 - 前記複合結合材生成用原料に含有される前記酸化アルミニウム成分が酸化アルミニウムであり、前記酸化アルミニウムの平均粒子径が、下限値2.5μm、上限値15.0μmである請求項13に記載の多孔質材料の製造方法。
- 前記複合結合材生成用原料に含有される前記酸化アルミニウムが、α−アルミナである請求項14に記載の多孔質材料の製造方法。
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