JP2018030105A - 多孔質セラミックス構造体 - Google Patents
多孔質セラミックス構造体 Download PDFInfo
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- JP2018030105A JP2018030105A JP2016165007A JP2016165007A JP2018030105A JP 2018030105 A JP2018030105 A JP 2018030105A JP 2016165007 A JP2016165007 A JP 2016165007A JP 2016165007 A JP2016165007 A JP 2016165007A JP 2018030105 A JP2018030105 A JP 2018030105A
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- Prior art keywords
- cerium dioxide
- porous ceramic
- oxide
- iron oxide
- ceramic structure
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 110
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 110
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000011148 porous material Substances 0.000 claims abstract description 23
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims description 31
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 12
- 229910052878 cordierite Inorganic materials 0.000 claims description 8
- 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 7
- 229910044991 metal oxide Inorganic materials 0.000 claims description 7
- 150000004706 metal oxides Chemical class 0.000 claims description 6
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 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 2
- 239000003054 catalyst Substances 0.000 abstract description 27
- 230000000694 effects Effects 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 21
- 238000005192 partition Methods 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 17
- 230000003197 catalytic effect Effects 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- 238000001179 sorption measurement Methods 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 239000006104 solid solution Substances 0.000 description 10
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 9
- 238000010304 firing Methods 0.000 description 9
- 238000000576 coating method Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000000746 purification Methods 0.000 description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- 239000004927 clay Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000002485 combustion reaction 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
- 238000007598 dipping method Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 230000001771 impaired effect Effects 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
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 metal oxide nitrate Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- UFQXGXDIJMBKTC-UHFFFAOYSA-N oxostrontium Chemical compound [Sr]=O UFQXGXDIJMBKTC-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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Abstract
Description
(1)坏土の調製
表1に示すハニカム構造体の骨材、酸化物含有二酸化セリウム(二酸化セリウム+鉄酸化物)を秤量し、ニーダーを用いて15分間乾式混合した後、水を投入し、ニーダーを用いて更に30分間混練して坏土を得た。このとき、二酸化セリウムの添加量及び添加有無、二酸化セリウムに対する鉄酸化物の比率等を変化させ、上記表1の実施例1〜5及び比較例1〜3に沿った坏土をそれぞれ形成する。なお、酸化物含有二酸化セリウムは、既に説明した含浸法等を用い、二酸化セリウムに鉄酸化物を含浸し、更に焼成処理をすることで鉄酸化物の一部が二酸化セリウムに固溶または付着したものが予め準備されている。なお、坏土の調製は、上記の通り、酸化物含有二酸化セリウムを予め準備するものに限定されず、例えば、ハニカム構造体の骨材に、二酸化セリウム、鉄酸化物(または、硝酸鉄溶液)を混合したものを坏土としてもよい。
実施例及び比較例毎にそれぞれ調製された複数種の坏土を、真空土練機を使用して柱状に成形した後、押出成形機に導入してハニカム状のハニカム成形体を押出成形する。なお、ハニカム成形体は、ハニカム径が30mm、隔壁厚さが12mil(約0.3mm)、セル密度が300cpsi(cell per square inches:46.5セル/cm2)、外周壁厚さが約0.6mmであり、内部に流体の流路となる複数のセルを区画形成する格子状の隔壁を備えたものである。
作製されたハニカム成形体をマイクロ波乾燥によって約70%の水分を蒸散させた後、熱風乾燥(80℃×12時間)する。その後、450℃を維持する脱媒炉に投入し、ハニカム成形体に残留する有機物成分を除去する脱脂を行い、その後、焼成温度を1450℃に設定し、アルゴン雰囲気圧下で焼成処理(本焼成)を行う。その後、詳細温度を1250℃に設定し、大気圧下で酸化処理を行う。これにより、構造体内部に二酸化セリウム及び鉄酸化物を有する酸化物含有二酸化セリウムを含んだハニカム構造体が形成される。
上記によって得られたハニカム構造体の試料(実施例1〜5、比較例1〜3)に対し、基材成分の比率、二酸化セリウム及び鉄酸化物の比率、二酸化セリウムの粒子径、二酸化セリウム粒子の比表面積、鉄酸化物粒子の比表面積、各粒子の結晶相を測定した。以下に、分析及び算出の具体的な方法を示す。
各成分の質量%は、それぞれICP発光分光分析法(Inductivity Coupled Plasma Atomic Emission Spectroscopy)に基づき分析を行うことで算出した。
ハニカム構造体の比表面積は、周知のBET法により測定を行った。更に、二酸化セリウムの平均粒子径は、レーザー回折法によって算出したメジアン径とした。なお、平均粒子径は、上記レーザー回折法以外にも、例えば、走査型電子顕微鏡(SEM)によって観察された視野像内の二酸化セリウム6の個々の粒子について、視野像内のサイズ及び拡大倍率に基づいて粒子径を算出し、その平均値を平均粒子径として算出したものであってもよい。なお、酸化物含有二酸化セリウムを有するハニカム構造体の場合(実施例1〜5)の比表面積は、当該酸化物含有二酸化セリウムを有しないハニカム構造体(比較例1)の比表面積が高くなっている(表1参照)。すなわち、酸化物含有二酸化セリウムが存在が、ハニカム構造体の比表面積を増大させる要因となっている。
各粒子の結晶相は、作成された試料に対し、X線回折装置(回転対陰極型X線回折装置:理学電機製、RINT)を用いて測定した。ここで、X線回折測定の条件は、CuKα源、50kV、300mA、2θ=10〜60°とし、得られたX線回折データを市販のX線データ解析ソフトを用いて解析した。
NO吸着量は、NOガスを用いた昇温脱離法に基づいて算出した。ここで、NO吸着量の算出のための装置として、AutoChemII(Micromeritis社製)を用いた。更に吸着に用いるガスとして、200pmNO、10%O2、Heの混合ガスを使用した。昇温炉内の反応管内に上記測定試料を載置し、ガス吸着時の温度が250℃となるように設定し、上記ガスを反応管内に導入した。吸着時間は30分とした。吸着完了後、反応管内にHeガスを導入し、昇温速度を10℃/minに設定した条件で、250〜600℃まで昇温を行った。昇温時における脱ガス成分を質量分析計によって計測し、NO脱離量を算出した。係るNO脱離量をNO吸着量とした。
上記1によって作成されたハニカム触媒体を、それぞれ直径25.4mm×長さ50.8mmの試験片に加工し、加工した外周をコート処理した。得られた試験片を測定試料として、自動車排ガス分析装置(SIGU1000:HORIBA社製)を用いて評価を行った。このとき、昇温炉内の反応管内に上記測定試料を載置し、測定試料が250℃になるまで暖めた。そして、200ppmNO(一酸化窒素)、10%O2(酸素)、及びN2(窒素)の混合ガスを反応ガスとして、反応管内に導入した。このとき、測定試料から排出された排出ガス(出口ガス)を排ガス測定装置(MEXA−6000FT:HORIBA社製)を用いて分析し、それぞれの排出濃度(NO濃度、NO2濃度)を測定した。更に、排出濃度の測定結果に基づいて、NO2変換率を求めた。ここで、NO2変換率は、(1−(NO濃度/(NO濃度+NO2濃度)))により算出される。
算出されたNO2変換率の値が1.0%以上のものを“A”、0.5%以上、1.0%未満のものを“B”、0.1%以上、0.5%未満のものを“C”、及び、0.1%未満のものを“D”として評価した。ここで、NO2変換率の値がD評価の0.1%未満の場合、上記自動車ガス分析装置による測定誤差を考慮し、ほとんどNO2変換がされていないものと判断される。実用上は、少なくともC評価以上が必要とされる。
上記表1及び表2に示されるように、二酸化セリウムの平均粒子径が小さくなるにつれて、NO吸着量やNO2変換率の評価が良好になることが示され、その平均粒子径は二酸化セリウムの含有量に依存することが確認された。特に、実施例2のハニカム構造体が良好な結果を示している。これに対し、比較例1のように酸化物含有二酸化セリウムを有しないハニカム構造体の場合には、NO吸着量の値が0であり、NO2変換率もD評価であることが確認された。また、比較例2のように鉄酸化物を含有しない二酸化セリウムのみを備えるハニカム構造体でもほとんど効果が認められなかった。加えて、最も高い効果の得られた実施例2と二酸化セリウムの比率が同じ比較例4でも、ディッピングにより担持された場合はNO吸着量及びNO2変換率の評価が低くなることが示された。
Claims (8)
- セラミックス材料で形成され、構造体内部に気孔を有する多孔質セラミックス構造体であって、
前記多孔質セラミックス構造体は、
二酸化セリウムを有し、
前記二酸化セリウムの少なくとも一部は、前記構造体内部に取り込まれ、かつ、前記気孔の気孔表面に少なくとも一部が露出しており、露出した前記二酸化セリウムの少なくとも一部は、表面及び/または内部に鉄酸化物を備える多孔質セラミックス構造体。 - 前記鉄酸化物は、
前記二酸化セリウムに固溶している請求項1に記載の多孔質セラミックス構造体。 - 前記二酸化セリウムの平均粒子径は、
0.1μm〜1.0μmの範囲である請求項1または2に記載の多孔質セラミックス構造体。 - 前記セラミックス材料に占める前記二酸化セリウムの比率は、
0.1質量%〜5.0質量%の範囲である請求項1〜3のいずれか一項に記載の多孔質セラミックス構造体。 - 前記セラミックス材料に占める前記鉄酸化物の比率は、
0.02質量%〜0.6質量%の範囲である請求項1〜4のいずれか一項に記載の多孔質セラミックス構造体。 - 前記二酸化セリウムは、
前記鉄酸化物とともに、マンガン、ストロンチウム、及びアルミニウムの少なくともいずれか一つの金属酸化物を更に備える請求項1〜5のいずれか一項に記載の多孔質セラミックス構造体。 - 前記セラミックス材料は、
コージェライト、または珪素−炭化珪素のいずれか一方を主成分とする請求項1〜6のいずれか一項に記載の多孔質セラミックス構造体。 - 前記多孔質セラミックス構造体は、
ハニカム構造体である請求項1〜7のいずれか一項に記載の多孔質セラミックス構造体。
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DE102021203079A1 (de) | 2020-03-27 | 2021-09-30 | Ngk Insulators, Ltd. | Poröse Keramikstruktur und Verfahren zur Herstellung einer porösen Keramikstruktur |
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JP7191985B2 (ja) | 2019-01-21 | 2022-12-19 | 日本碍子株式会社 | 多孔質セラミック構造体 |
JPWO2020153156A1 (ja) * | 2019-01-21 | 2021-10-21 | 日本碍子株式会社 | 多孔質セラミック構造体 |
US11480081B2 (en) | 2019-01-21 | 2022-10-25 | Ngk Insulators, Ltd. | Porous ceramic structure |
WO2020153156A1 (ja) * | 2019-01-21 | 2020-07-30 | 日本碍子株式会社 | 多孔質セラミック構造体 |
DE112020000288T5 (de) | 2019-01-21 | 2021-10-14 | Ngk Insulators, Ltd. | Poröse Keramikstruktur |
US11666890B2 (en) | 2019-03-14 | 2023-06-06 | Ngk Insulators, Ltd. | Porous ceramic structure |
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JP7181820B2 (ja) | 2019-03-14 | 2022-12-01 | 日本碍子株式会社 | 多孔質セラミック構造体 |
JP2021155276A (ja) * | 2020-03-27 | 2021-10-07 | 日本碍子株式会社 | 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 |
US11819830B2 (en) | 2020-03-27 | 2023-11-21 | Ngk Insulators, Ltd. | Porous ceramic structure and method of producing porous ceramic structure |
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JP2021155277A (ja) * | 2020-03-27 | 2021-10-07 | 日本碍子株式会社 | 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 |
DE102021203078A1 (de) | 2020-03-27 | 2021-09-30 | Ngk Insulators, Ltd. | Poröse Keramikstruktur und Verfahren zum Herstellen einer porösen Keramikstruktur |
US11731111B2 (en) | 2020-03-27 | 2023-08-22 | Ngk Insulators, Ltd. | Porous ceramic structure and method of producing porous ceramic structure |
CN113441149B (zh) * | 2020-03-27 | 2023-08-22 | 日本碍子株式会社 | 多孔质陶瓷结构体及多孔质陶瓷结构体的制造方法 |
JP7379248B2 (ja) | 2020-03-27 | 2023-11-14 | 日本碍子株式会社 | 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 |
JP7379247B2 (ja) | 2020-03-27 | 2023-11-14 | 日本碍子株式会社 | 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 |
DE102021203079A1 (de) | 2020-03-27 | 2021-09-30 | Ngk Insulators, Ltd. | Poröse Keramikstruktur und Verfahren zur Herstellung einer porösen Keramikstruktur |
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JP6692256B2 (ja) | 2020-05-13 |
DE102017006390A1 (de) | 2018-03-01 |
CN107778022A (zh) | 2018-03-09 |
CN107778022B (zh) | 2021-12-14 |
US20180057407A1 (en) | 2018-03-01 |
DE102017006390B4 (de) | 2019-05-09 |
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