JPWO2012128149A1 - 炭化珪素質多孔体、ハニカム構造体及び電気加熱式触媒担体 - Google Patents
炭化珪素質多孔体、ハニカム構造体及び電気加熱式触媒担体 Download PDFInfo
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- silicon carbide
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- carbide based
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 83
- 239000003054 catalyst Substances 0.000 title claims description 18
- 239000011148 porous material Substances 0.000 claims abstract description 70
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 32
- 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 group [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 abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 21
- 239000010703 silicon Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 description 22
- 238000012360 testing method Methods 0.000 description 20
- 230000035939 shock Effects 0.000 description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002994 raw material Substances 0.000 description 16
- 230000020169 heat generation Effects 0.000 description 14
- 230000003197 catalytic effect Effects 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- 239000004927 clay Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 239000011863 silicon-based powder Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000010304 firing Methods 0.000 description 8
- 238000005485 electric heating Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000005192 partition Methods 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 238000007561 laser diffraction method Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 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
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 235000010980 cellulose Nutrition 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000007604 dielectric heating drying Methods 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000007602 hot air drying Methods 0.000 description 2
- -1 hydroxypropoxyl Chemical group 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229910001753 sapphirine Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000004901 spalling Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
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- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
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- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
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- 230000015556 catabolic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
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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
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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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
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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Abstract
Description
開気孔率[%]=全細孔容積/{(1/見掛け密度)+全細孔容積} ×100
強度=ハニカム構造体の曲げ強度/{1−(開口率/100)}
炭化珪素(SiC)粉末と金属珪素(Si)粉末とコーディエライト粒子を64:28:8の質量割合で混合した。この混合物に、バインダー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。この成形原料を混練し、土練して円柱状の坏土を作製した。バインダーの含有量はSiC粉末とSi粉末の合計に対し7質量%であり、造孔材の含有量はSiC粉末とSi粉末の合計に対し2質量%であり、水の含有量はSiC粉末とSi粉末の合計に対し35質量%であった。SiC粉末の平均粒子径は30μmであり、Si粉末の平均粒子径は6μmであった。また、造孔材の平均粒子径は、20μmであった。なお、SiC粒子、Si粒子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。
・組成
ハニカム構造の炭化珪素質多孔体の組成は、粉末X線回折の内部標準法により測定した。なお、原料の組成比と炭化珪素質多孔体の組成比とのズレは1%程度であった。
・開気孔率
水銀圧入法(JIS R 1655準拠)による全細孔容積[cm3/g]と気相置換法による乾式自動密度測定機による見掛密度[g/cm3]から、下記式にて算出した。
開気孔率[%]=全細孔容積/{(1/見掛密度)+全細孔容積}×100
・平均気孔径
水銀圧入法(JIS R 1655準拠)により測定した。
・強度
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5セル×横10セル×長さ40mm)に加工し、JIS R1601に準拠した曲げ試験によりハニカム構造体の曲げ強度を算出した後、別途計測したハニカムの開口率を用いて、下記式にて算出した。
強度=ハニカム構造体の曲げ強度/{1−(開口率/100)}
・熱伝導率
比熱と熱拡散率と嵩密度の積として算出した。なお、比熱はDSC法、熱拡散率は光交流法により測定した。また、嵩密度は下記式から算出した。
嵩密度=1/{(1/見掛密度)+全細孔容積}
・平均線熱膨張係数
JIS R1618に準拠して、室温〜800℃の平均線熱膨張係数を測定した。
・体積抵抗率
室温で4端子法により測定した。
・通電発熱試験
実施例1と同じ組成の原料を用いて、別途、板状の成形体を作製し、その成形体に上述した乾燥・脱脂・焼成・酸化処理を施し、板状の焼成体とし、その焼成体から縦30mm×横40mm×厚さ0.3mmの試験片を切り出した。その試験片の一方の長辺の頂点を電極として、1Vから500Vへ徐々に電圧を上げながら通電し、試験片の温度分布の時間変化をサーモグラフィーで測定した。このとき、電極間の中点の温度が200℃となった時点での試験片の中心部と電極間の中点の温度(200℃)との差をΔTとした。ΔTが80℃未満のとき「◎」、80℃以上〜120℃未満のとき「○」、120℃以上のとき「△」とした。つまり、「◎」、「○」、「△」は、試験片の温度分布の均一性を表す指標であり、「◎」や「○」は温度分布が比較的均一であることを示し、「△」は温度分布にムラがあることを示す。また、「×」は抵抗が高すぎて電流が流れなかったことを示す。なお、体積抵抗率の高い比較例2,4では、電圧を上げていってもなかなか電流が流れず、高電圧になったとき、一気に電流が流れて電極間中点温度は急激に上昇したが、そのときの試料中心部への熱の伝わりが遅いため、ΔTは大きくなった。
・電気炉スポーリング試験(急速冷却試験)
ハニカム構造体を電気炉にて所定温度で2h加熱し、均一な温度にした後、室温に取り出し、クラックの発生の有無を目視で観察した。このとき、所定温度を650℃としたときにクラックが発生しなかったものを「○」、650℃としたときにクラックが発生したものを「△」、それ以下の温度でクラックが発生したものを「×」とした。クラックが発生する温度が高いものほど耐熱衝撃性が高いことを示す。
実施例2〜17,比較例1〜5は、表1に記載の組成とすることと、造孔材量や原料の平均粒径を微調整した以外は、実施例1に準じて炭化珪素質多孔体を製造した。なお、炭化珪素質多孔体の組成の測定結果から、実施例1〜17の酸化物相は、コーディエライトであった。ただし、ごく僅かな異相(ムライト、クリストバライト、スピネル、サフィリンなど)も存在した。比較例1〜3のコーディエライトを含まない酸化物相の主成分は、SrO−SiO2であった。
Claims (6)
- 炭化珪素粒子と、金属珪素と、酸化物相とを含み、前記炭化珪素粒子どうしが前記金属珪素及び前記酸化物相の少なくとも一方を介して結合されている炭化珪素質多孔体であって、
前記酸化物相の主成分がコーディエライトであり、開気孔率が10〜40%である、
炭化珪素質多孔体。 - 室温における体積抵抗率が1〜80Ωcm、熱伝導率が30〜70W/m・Kである、
請求項1に記載の炭化珪素質多孔体。 - 炭化珪素を50〜80重量%、金属珪素を15〜40重量%、コーディエライトを1〜25重量%含む、
請求項1又は2に記載の炭化珪素質多孔体。 - 前記金属珪素が前記酸化物相によって覆われている、
請求項1〜3のいずれか1項に記載の炭化珪素質多孔体。 - 請求項1〜4のいずれか1項に記載の炭化珪素質多孔体で構成される、ハニカム構造体。
- 請求項1〜4のいずれか1項に記載の炭化珪素質多孔体を利用した、電気加熱式触媒担体。
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JP6912412B2 (ja) * | 2018-03-30 | 2021-08-04 | 日本碍子株式会社 | 炭化珪素質多孔体及びその製造方法 |
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