JP7379248B2 - 多孔質セラミック構造体および多孔質セラミック構造体の製造方法 - Google Patents
多孔質セラミック構造体および多孔質セラミック構造体の製造方法 Download PDFInfo
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- JP7379248B2 JP7379248B2 JP2020057683A JP2020057683A JP7379248B2 JP 7379248 B2 JP7379248 B2 JP 7379248B2 JP 2020057683 A JP2020057683 A JP 2020057683A JP 2020057683 A JP2020057683 A JP 2020057683A JP 7379248 B2 JP7379248 B2 JP 7379248B2
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- 239000000919 ceramic Substances 0.000 title claims description 175
- 238000000034 method Methods 0.000 title claims description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 212
- 239000002245 particle Substances 0.000 claims description 192
- 239000011572 manganese Substances 0.000 claims description 122
- 229910044991 metal oxide Inorganic materials 0.000 claims description 108
- 150000004706 metal oxides Chemical class 0.000 claims description 108
- 229910052742 iron Inorganic materials 0.000 claims description 84
- 229910052684 Cerium Inorganic materials 0.000 claims description 64
- 239000010941 cobalt Substances 0.000 claims description 64
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 64
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 63
- 229910017052 cobalt Inorganic materials 0.000 claims description 63
- 229910052748 manganese Inorganic materials 0.000 claims description 59
- 239000011148 porous material Substances 0.000 claims description 54
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 46
- 238000010304 firing Methods 0.000 claims description 41
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 38
- 238000002425 crystallisation Methods 0.000 claims description 36
- 230000008025 crystallization Effects 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 35
- 229910052878 cordierite Inorganic materials 0.000 claims description 34
- 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 description 34
- 239000007791 liquid phase Substances 0.000 claims description 34
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 25
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 19
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 19
- 239000004927 clay Substances 0.000 claims description 17
- 229910052596 spinel Inorganic materials 0.000 claims description 17
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- 238000010438 heat treatment Methods 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 238000004898 kneading Methods 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 9
- 239000013618 particulate matter Substances 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 60
- 230000003197 catalytic effect Effects 0.000 description 37
- 238000012423 maintenance Methods 0.000 description 28
- 238000005192 partition Methods 0.000 description 23
- 238000006243 chemical reaction Methods 0.000 description 21
- 230000003647 oxidation Effects 0.000 description 17
- 238000007254 oxidation reaction Methods 0.000 description 17
- 230000008569 process Effects 0.000 description 17
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 16
- 229910002091 carbon monoxide Inorganic materials 0.000 description 16
- 239000000463 material Substances 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 12
- 239000012071 phase Substances 0.000 description 12
- 238000001878 scanning electron micrograph Methods 0.000 description 11
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- 239000013078 crystal Substances 0.000 description 9
- 238000000746 purification Methods 0.000 description 9
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 6
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- 230000007423 decrease Effects 0.000 description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 229910002089 NOx Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
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- 229910000510 noble metal Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 238000002276 dielectric drying Methods 0.000 description 1
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- 239000000446 fuel Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 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
- 238000007561 laser diffraction method Methods 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- 230000008929 regeneration Effects 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Description
2 金属酸化物粒子
3 セリウム含有粒子
10 ハニカム構造体
21 固定部
22 突出部
81 DPF
83 CSF
S11~S13,S21~S24 ステップ
Claims (9)
- 多孔質セラミック構造体であって、
主成分がコージェライトである多孔質の構造体本体と、
前記構造体本体に固定されたセリウム含有粒子と、
鉄、マンガンおよびコバルトのうち少なくとも1種を含むスピネル型構造を有する酸化物の粒子であり、前記構造体本体の気孔の内部に固定された金属酸化物粒子と、
を備え、
前記金属酸化物粒子は、
前記構造体本体の内部に位置する固定部と、
前記固定部に連続するとともに前記気孔内に突出する突出部と、
を備え、
前記多孔質セラミック構造体において、
鉄が含まれる場合の鉄の含有率は、Fe2O3換算で1.5質量%以上かつ3.0質量%以下であり、
マンガンが含まれる場合のマンガンの含有率は、Mn2O3換算で1.5質量%以上かつ3.0質量%以下であり、
鉄またはマンガンと共にコバルトが含まれる場合のコバルトの含有率は、Co3O4換算で1.5質量%以上かつ3.0質量%以下であり、
鉄およびマンガンは含まれずコバルトが含まれる場合のコバルトの含有率は、Co3O4換算で3.0質量%以上かつ6.0質量%以下であり、
セリウムの含有率は、CeO2換算で1.5質量%以上かつ4.5質量%以下であり、
CeO2換算でのセリウムの含有率に対する、Fe2O3換算での鉄の含有率とMn2O3換算でのマンガンの含有率とCo3O4換算でのコバルトの含有率との和の割合は、1.0以上かつ4.0以下であり、
前記金属酸化物粒子の含有率は、0.3質量%以上かつ8.0質量%以下であることを特徴とする多孔質セラミック構造体。 - 請求項1に記載の多孔質セラミック構造体であって、
前記金属酸化物粒子は、鉄、マンガンおよび酸素を含むスピネル型構造を有する酸化物の粒子、または、コバルトおよび酸素を含むスピネル型構造を有する酸化物の粒子であることを特徴とする多孔質セラミック構造体。 - 請求項1または2に記載の多孔質セラミック構造体であって、
前記金属酸化物粒子の平均粒径は、10nm以上かつ1μm以下であることを特徴とする多孔質セラミック構造体。 - 請求項1ないし3のいずれか1つに記載の多孔質セラミック構造体であって、
ディーゼルエンジンから排出される排ガス中の粒子状物質を捕集するディーゼル・パティキュレート・フィルタに使用されることを特徴とする多孔質セラミック構造体。 - 多孔質セラミック構造体の製造方法であって、
a)原料を混練して坏土を調製する工程と、
b)前記坏土を成形して成形体を得る工程と、
c)前記成形体を焼成する工程と、
を備え、
前記原料は、
コージェライトと、
セリウムと、
鉄、マンガンおよびコバルトのうち少なくとも1種と、
を含み、
前記c)工程により、主成分がコージェライトである多孔質の構造体本体と、前記構造体本体に固定されたセリウム含有粒子と、鉄、マンガンおよびコバルトのうち少なくとも1種を含むスピネル型構造を有する酸化物の粒子であり、前記構造体本体の気孔の内部に固定された金属酸化物粒子と、を備える多孔質セラミック構造体が形成され、
前記多孔質セラミック構造体において、
鉄が含まれる場合の鉄の含有率は、Fe 2 O 3 換算で1.5質量%以上かつ3.0質量%以下であり、
マンガンが含まれる場合のマンガンの含有率は、Mn 2 O 3 換算で1.5質量%以上かつ3.0質量%以下であり、
鉄またはマンガンと共にコバルトが含まれる場合のコバルトの含有率は、Co 3 O 4 換算で1.5質量%以上かつ3.0質量%以下であり、
鉄およびマンガンは含まれずコバルトが含まれる場合のコバルトの含有率は、Co 3 O 4 換算で3.0質量%以上かつ6.0質量%以下であり、
セリウムの含有率は、CeO 2 換算で1.5質量%以上かつ4.5質量%以下であり、
CeO 2 換算でのセリウムの含有率に対する、Fe 2 O 3 換算での鉄の含有率とMn 2 O 3 換算でのマンガンの含有率とCo 3 O 4 換算でのコバルトの含有率との和の割合は、1.0以上かつ4.0以下であり、
前記多孔質セラミック構造体は、ZnO換算で0.03質量%以上かつ2.5質量%以下の亜鉛を含み、
前記c)工程は、
c1)前記成形体を、液相生成温度以下の第1温度まで昇温する工程と、
c2)前記成形体を、前記第1温度から、前記液相生成温度よりも高くかつ前記金属酸化物粒子の結晶化温度未満の第2温度まで昇温する工程と、
c3)前記成形体を、前記第2温度から、前記結晶化温度よりも高くかつ最高温度以下の第3温度まで昇温する工程と、
c4)前記成形体を前記最高温度にて所定時間維持する工程と、
を備え、
前記c2)工程における昇温速度は、100℃/h以上かつ200℃/h以下であることを特徴とする多孔質セラミック構造体の製造方法。 - 請求項5に記載の多孔質セラミック構造体の製造方法であって、
前記c3)工程における昇温速度は、100℃/h以上かつ200℃/h以下であることを特徴とする多孔質セラミック構造体の製造方法。 - 多孔質セラミック構造体の製造方法であって、
a)原料を混練して坏土を調製する工程と、
b)前記坏土を成形して成形体を得る工程と、
c)前記成形体を焼成する工程と、
を備え、
前記原料は、
コージェライトと、
セリウムと、
鉄、マンガンおよびコバルトのうち少なくとも1種と、
を含み、
前記c)工程により、主成分がコージェライトである多孔質の構造体本体と、前記構造体本体に固定されたセリウム含有粒子と、鉄、マンガンおよびコバルトのうち少なくとも1種を含むスピネル型構造を有する酸化物の粒子であり、前記構造体本体の気孔の内部に固定された金属酸化物粒子と、を備える多孔質セラミック構造体が形成され、
前記多孔質セラミック構造体において、
鉄が含まれる場合の鉄の含有率は、Fe 2 O 3 換算で1.5質量%以上かつ3.0質量%以下であり、
マンガンが含まれる場合のマンガンの含有率は、Mn 2 O 3 換算で1.5質量%以上かつ3.0質量%以下であり、
鉄またはマンガンと共にコバルトが含まれる場合のコバルトの含有率は、Co 3 O 4 換算で1.5質量%以上かつ3.0質量%以下であり、
鉄およびマンガンは含まれずコバルトが含まれる場合のコバルトの含有率は、Co 3 O 4 換算で3.0質量%以上かつ6.0質量%以下であり、
セリウムの含有率は、CeO 2 換算で1.5質量%以上かつ4.5質量%以下であり、
CeO 2 換算でのセリウムの含有率に対する、Fe 2 O 3 換算での鉄の含有率とMn 2 O 3 換算でのマンガンの含有率とCo 3 O 4 換算でのコバルトの含有率との和の割合は、1.0以上かつ4.0以下であり、
前記多孔質セラミック構造体は、ZnO換算で0.03質量%以上かつ2.5質量%以下の亜鉛を含み、
前記c)工程は、
c1)前記成形体を、液相生成温度以下の第1温度まで昇温する工程と、
c2)前記成形体を、前記第1温度から、前記液相生成温度よりも高くかつ前記金属酸化物粒子の結晶化温度未満の第2温度まで昇温する工程と、
c3)前記成形体を、前記第2温度から、前記結晶化温度よりも高くかつ最高温度以下の第3温度まで昇温する工程と、
c4)前記成形体を前記最高温度にて所定時間維持する工程と、
を備え、
前記c2)工程における昇温速度は、1℃/h以上かつ10℃/h以下であることを特徴とする多孔質セラミック構造体の製造方法。 - 請求項5ないし7のいずれか1つに記載の多孔質セラミック構造体の製造方法であって、
前記c3)工程において、前記成形体が前記結晶化温度にて所定時間維持されることを特徴とする多孔質セラミック構造体の製造方法。 - 多孔質セラミック構造体の製造方法であって、
a)原料を混練して坏土を調製する工程と、
b)前記坏土を成形して成形体を得る工程と、
c)前記成形体を焼成する工程と、
を備え、
前記原料は、
コージェライトと、
セリウムと、
鉄、マンガンおよびコバルトのうち少なくとも1種と、
を含み、
前記c)工程により、主成分がコージェライトである多孔質の構造体本体と、前記構造体本体に固定されたセリウム含有粒子と、鉄、マンガンおよびコバルトのうち少なくとも1種を含むスピネル型構造を有する酸化物の粒子であり、前記構造体本体の気孔の内部に固定された金属酸化物粒子と、を備える多孔質セラミック構造体が形成され、
前記多孔質セラミック構造体において、
鉄が含まれる場合の鉄の含有率は、Fe 2 O 3 換算で1.5質量%以上かつ3.0質量%以下であり、
マンガンが含まれる場合のマンガンの含有率は、Mn 2 O 3 換算で1.5質量%以上かつ3.0質量%以下であり、
鉄またはマンガンと共にコバルトが含まれる場合のコバルトの含有率は、Co 3 O 4 換算で1.5質量%以上かつ3.0質量%以下であり、
鉄およびマンガンは含まれずコバルトが含まれる場合のコバルトの含有率は、Co 3 O 4 換算で3.0質量%以上かつ6.0質量%以下であり、
セリウムの含有率は、CeO 2 換算で1.5質量%以上かつ4.5質量%以下であり、
CeO 2 換算でのセリウムの含有率に対する、Fe 2 O 3 換算での鉄の含有率とMn 2 O 3 換算でのマンガンの含有率とCo 3 O 4 換算でのコバルトの含有率との和の割合は、1.0以上かつ4.0以下であり、
前記多孔質セラミック構造体は、ZnO換算で0.03質量%以上かつ2.5質量%以下の亜鉛を含み、
前記c)工程は、
c1)前記成形体を、液相生成温度以下の第1温度まで昇温する工程と、
c2)前記成形体を、前記第1温度から、前記液相生成温度よりも高くかつ前記金属酸化物粒子の結晶化温度未満の第2温度まで昇温する工程と、
c3)前記成形体を、前記第2温度から、前記結晶化温度よりも高くかつ最高温度以下の第3温度まで昇温する工程と、
c4)前記成形体を前記最高温度にて所定時間維持する工程と、
を備え、
前記c3)工程において、前記成形体が前記結晶化温度にて所定時間維持されることを特徴とする多孔質セラミック構造体の製造方法。
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