WO2022202903A1 - 炭化珪素質セラミックハニカム構造体及びその製造方法 - Google Patents
炭化珪素質セラミックハニカム構造体及びその製造方法 Download PDFInfo
- Publication number
- WO2022202903A1 WO2022202903A1 PCT/JP2022/013530 JP2022013530W WO2022202903A1 WO 2022202903 A1 WO2022202903 A1 WO 2022202903A1 JP 2022013530 W JP2022013530 W JP 2022013530W WO 2022202903 A1 WO2022202903 A1 WO 2022202903A1
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- Prior art keywords
- particles
- silicon carbide
- ceramic honeycomb
- honeycomb structure
- phase
- Prior art date
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 65
- 239000000919 ceramic Substances 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000002245 particle Substances 0.000 claims abstract description 109
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 39
- 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 abstract description 39
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 22
- 239000011029 spinel Substances 0.000 claims abstract description 22
- 238000005192 partition Methods 0.000 claims abstract description 19
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 91
- 239000000395 magnesium oxide Substances 0.000 claims description 49
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 45
- 239000011148 porous material Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 30
- 239000011230 binding agent Substances 0.000 claims description 23
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 239000004927 clay Substances 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims 1
- 238000010304 firing Methods 0.000 description 29
- 239000007789 gas Substances 0.000 description 19
- 230000001590 oxidative effect Effects 0.000 description 13
- 230000035939 shock Effects 0.000 description 13
- 238000005245 sintering Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 230000001186 cumulative effect Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 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 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 3
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 3
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 3
- 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 3
- 238000005304 joining Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910019440 Mg(OH) Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229910052839 forsterite Inorganic materials 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
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- 239000013618 particulate matter Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
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- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 229920013819 hydroxyethyl ethylcellulose Polymers 0.000 description 1
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- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
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- 238000001953 recrystallisation Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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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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- F01N2370/00—Selection of materials for exhaust purification
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Definitions
- the present invention removes particulate matter (Particulate Matter (hereinafter sometimes referred to as "PM")) in the exhaust gas emitted from internal combustion engines such as diesel engines, etc., and purifies the exhaust gas.
- PM particulate Matter
- the present invention relates to a silicon carbide ceramic honeycomb structure used in a honeycomb filter and a manufacturing method thereof.
- the NOx and PM contained in the exhaust gas of diesel engines can have a negative impact on the human body and the environment if they are released into the atmosphere.
- a structure and a ceramic honeycomb filter for trapping PM are attached.
- An example of a ceramic honeycomb filter for collecting PM in exhaust gas and purifying the exhaust gas is shown in FIGS. 1(a) and 1(b).
- the ceramic honeycomb filter 100 includes a ceramic honeycomb structure 110 composed of porous partition walls 12 forming a plurality of channels 13 and 14 and an outer peripheral wall 11, an outflow-side plugged channel 13 and an inflow-side plugged channel 14.
- the exhaust gas flows from the outflow-side sealed flow path 13 opening at the exhaust gas inflow-side end face 15a, and passes through the communication holes present on the surface and inside of the partition wall 12. and is discharged from the inflow-side sealed channel 14 opening at the outflow-side end surface 15b.
- the exhaust gas passes through the communicating holes present on the surface and inside of the partition wall 12, PM in the exhaust gas is captured and the exhaust gas is purified.
- the collected PM is burned and regenerated when the accumulated amount reaches a predetermined amount.
- Such ceramic honeycomb structures are used in increasingly harsh environments, and it is known to use refractory particles such as silicon carbide (SiC) particles, which are excellent in thermal shock resistance, as their constituent materials.
- Patent Document 1 uses silicon carbide powder having a specific surface area of 0.1 to 5 m 2 /g and an impurity component of 1.0 to 5.0% as a starting material, which is molded into a desired shape and dried. Later, it discloses a method of producing a catalyst carrier by sintering at a temperature in the range of 1600 to 2200°C. It states.
- JP-A-6-182228 is a method of forming a sintered body using only silicon carbide powder as a starting material. Particles are bound together. Therefore, a very high firing temperature is required to form a fired body, and if a filter with a high porosity is to be manufactured, this sintering mechanism will not function sufficiently, resulting in a decrease in strength. There is In addition, since this method is a sintering method in which silicon carbide particles are bonded to each other by a recrystallization reaction of the silicon carbide powder itself, a very high firing temperature is required, resulting in high cost.
- Patent Document 2 Japanese Patent Application Laid-Open No. 2002-201082 (Patent Document 2) can be manufactured at a relatively low firing temperature at a low cost, and has a high porosity that is sufficient to keep the pressure loss low when used as an automobile exhaust gas filter.
- the following method is disclosed as a method for manufacturing a honeycomb structure having thermal conductivity. That is, Japanese Patent Application Laid-Open No. 2002-201082 discloses that a clay obtained by adding metal silicon and an organic binder to silicon carbide particles, mixing and kneading them, and molding them into a honeycomb shape, and calcining the obtained molded body. Disclosed is a method of manufacturing a honeycomb structure by removing the organic binder in the molded body and then firing it. The firing temperature is in the range of 1400 to 1600 ° C. It is described that a non-oxidizing atmosphere such as N 2 or Ar is preferable in a temperature range above the temperature at which the temperature starts.
- a non-oxidizing atmosphere such as N 2 or
- the honeycomb is sintered at a relatively low firing temperature of 1400 to 1600°C to ensure a sufficient porosity to keep the pressure loss low when used as a filter.
- a structure can be obtained, it is desirable to perform firing in a non-oxidizing atmosphere in order to suppress oxidation, leading to high costs for firing equipment.
- Patent Document 3 discloses a silicon carbide honeycomb structure having high porosity, high strength, and excellent thermal shock resistance, which is useful as a filter for which higher exhaust gas permeability is required. The following method is disclosed as a manufacturing method of. That is, Japanese Patent Application Laid-Open No. 2002-201082 discloses that a raw material mixture containing metal, silicon, carbon raw material and aluminum (Al) raw material is formed into a predetermined shape, degreased and fired to obtain 1 to 35% by mass of metal silicide and 0.5% by mass.
- JP-A-2010-105861 sintering is performed at a relatively low temperature of 1250 to 1800° C. to obtain a silicon carbide-based porous body having excellent gas permeability and thermal shock resistance. Since it is necessary to perform firing in an atmosphere or a vacuum atmosphere, the cost of firing equipment is increased.
- Patent Document 4 discloses an aggregate composed of a main aggregate composed of silicon carbide particles and a sub aggregate composed of at least one of mullite particles and alumina particles, and bonding the aggregates together. , a binder phase consisting of at least one of an amorphous phase and a cordierite phase, and a porous material having a porosity of 40 to 90%, forming a honeycomb structure with improved thermal shock resistance.
- JP-A-2002-201082 is prepared by mixing silicon carbide powder as a main aggregate, powder as a sub-aggregate, and powder as a binding phase (binder powder), and if necessary Then, a binder, a surfactant, a pore-forming material, water, etc. are added to prepare a forming raw material, kneaded to form a clay, extruded to form a honeycomb formed body, dried and fired. can get.
- JP-A-2002-201082 describes that the firing is preferably carried out at 1300-1600° C. in a non-oxidizing atmosphere such as nitrogen or argon.
- an object of the present invention is to maintain the thermal shock resistance of a ceramic honeycomb structure used in a ceramic honeycomb filter, while using a firing process that does not require a firing temperature and a non-oxidizing atmosphere that are relatively lower than those of the prior art.
- Another object of the present invention is to provide a silicon carbide ceramic honeycomb structure that can be manufactured at a lower cost than conventional ones, and a method for manufacturing the same.
- the present inventors have attempted to maintain the thermal shock resistance of a ceramic honeycomb structure even when using a firing process that does not require a firing temperature that is relatively low and a non-oxidizing atmosphere.
- the present invention was conceived as a result of intensive studies focusing on the raw material particles to be blended.
- the partition walls preferably have a porosity of 35 to 50%.
- the partition walls preferably have a median pore diameter of 5 to 20 ⁇ m.
- the method of the present invention for producing a silicon carbide ceramic honeycomb structure is obtained by blending, mixing, and kneading silicon carbide particles, a binder containing at least alumina source particles and magnesia source particles, and an organic binder.
- the kneaded clay is extruded into a honeycomb shape, and the obtained molded body is dried and then fired at a temperature of 1200 to 1350° C. in an air atmosphere.
- the method for producing a silicon carbide ceramic honeycomb structure of the present invention it is preferable to blend 6 to 15% by mass of the alumina source particles and the magnesia source particles in total with respect to 100% by mass of the silicon carbide particles.
- the alumina source particles of the binder are alumina particles or aluminum hydroxide particles
- the magnesia source particles are magnesium oxide particles or magnesium hydroxide particles.
- the present invention while maintaining thermal shock resistance as a ceramic honeycomb structure used for a ceramic honeycomb filter, a firing process that does not require a firing temperature and a non-oxidizing atmosphere that are relatively lower than those of the prior art is used. It is possible to provide a silicon carbide ceramic honeycomb structure that can be manufactured at a lower cost, and a method for manufacturing the same.
- FIG. 1 is a front view schematically showing an example of a ceramic honeycomb filter
- FIG. 2 is a partial cross-sectional view parallel to the axial direction schematically showing an example of a ceramic honeycomb filter
- 1 is a perspective view schematically showing a ceramic honeycomb segment
- FIG. 1 is a perspective view schematically showing an example of a ceramic honeycomb filter formed by joining and integrating;
- the molar ratio M1 of the cordierite phase is obtained from [cordierite phase (mol)/(cordierite phase (mol) + spinel phase ( mol))]. If the molar ratio M1 of the cordierite phase is less than 0.4, the strength is lowered and the coefficient of thermal expansion is increased to deteriorate the thermal shock resistance.
- the cordierite phase molar ratio M1 of the cordierite phase exceeds 0.9, the heat resistance is lowered and the porosity of the partition walls is lowered.
- the cordierite phase molar ratio M1 is preferably between 0.45 and 0.70.
- the bonding layer may contain other crystalline phases such as cristobalite, mullite, and forsterite, and amorphous phases in addition to cordierite and spinel phases.
- the porosity of the partition walls when the porosity of the partition walls is 35 to 50%, the pressure loss of the silicon carbide ceramic honeycomb structure can be kept low and the strength can be maintained. If the porosity is less than 35%, the pressure loss of the ceramic honeycomb structure will increase, while if it exceeds 50%, it will be difficult to obtain sufficient strength.
- the lower limit of porosity is preferably 38%, more preferably 40%.
- the upper limit of porosity is preferably 49%, more preferably 48%.
- the partition walls have a median pore diameter of 5 to 20 ⁇ m, so that the strength of the silicon carbide ceramic honeycomb structure can be maintained.
- the lower limit of the median pore size is preferably 8 ⁇ m, more preferably 9 ⁇ m.
- the upper limit of the median pore size is preferably 18 ⁇ m, more preferably 16 ⁇ m.
- the silicon carbide ceramic honeycomb structure of the present invention is used as honeycomb segments 211, and as shown in FIG. A silicon ceramic honeycomb structure 210 may be used.
- the plurality of honeycomb segments 211 are joined and integrated by the joining material layer 29, they are processed so that the outer peripheral shape of the cross section perpendicular to the flow path is circular, elliptical, triangular, square, or any other desired shape.
- the outer peripheral surface is coated with a coating material to form the outer peripheral wall 21 .
- the exhaust gas inflow side 25a or the exhaust gas outflow side 25b of the channel of the silicon carbide ceramic honeycomb structure 210 formed by joining and integrating is plugged alternately in a checkered pattern by a known method to form a ceramic honeycomb. It can be filter 200 .
- the sealing portions 26a and 26b formed in the flow paths may be formed in the molded body before firing or the fired honeycomb segments before being joined, or may be formed in the bonding material layer 29. It may be formed after joining and integrating. These sealing portions may be formed on the exhaust gas inflow side or exhaust gas outflow side end face portion of the flow path, or may be formed at a position inside the flow path from the inflow side end face 25a or the outflow side end face 26b. good too.
- silicon carbide particles as an aggregate, a binder containing at least alumina source particles and magnesia source particles, and an organic binder are blended and mixed.
- the alumina source particles and magnesia source particles refer to particles of a compound containing alumina and particles of a compound containing magnesia, respectively, and further include particles of a compound containing alumina and magnesia.
- the silicon carbide particles are contained as an aggregate, and the aggregates are bonded to each other via a bonding layer so as to form pores.
- Silicon carbide particles preferably have an average particle size of 30 to 50 ⁇ m.
- the bonding layer can contain at least a cordierite phase and a spinel phase.
- the molar ratio M2 is determined by calculation as follows from the masses of the blended alumina source particles and magnesia source particles.
- the lower limit of the molar ratio M2 is preferably 0.35, more preferably 0.40.
- the upper limit is preferably 0.48.
- alumina source particles and magnesia source particles in total with respect to 100% by mass of silicon carbide particles. If the content is less than 6% by mass, the bonding strength of the bonding layer that bonds the silicon carbide particles together will decrease, and the strength of the ceramic honeycomb structure will decrease. On the other hand, if it exceeds 15% by mass, the thermal shock resistance is lowered.
- the lower limit of the sum of the alumina source particles and the magnesia source particles is preferably 7% by mass, more preferably 8% by mass with respect to 100% by mass of the silicon carbide particles.
- the upper limit is preferably 14% by mass, more preferably 13% by mass.
- the average particle size of the alumina source particles is preferably 1-15 ⁇ m. Moreover, the average particle size of the magnesia source particles is preferably 1 to 15 ⁇ m.
- the alumina source particles are preferably alumina particles or aluminum hydroxide particles, and the magnesia source particles are preferably magnesium oxide particles or magnesium hydroxide particles.
- alumina particles or aluminum hydroxide particles as the alumina source particles and magnesium oxide particles or magnesium hydroxide particles as the magnesia source particles, as will be described later, a lower firing temperature than before and a non-oxidizing atmosphere are required. It is preferable because it becomes possible to bake without It is particularly preferred to use alumina particles as the alumina source particles and magnesium hydroxide particles as the magnesia source particles as binders.
- the binder in addition to these alumina source particles and magnesia source particles, spinel particles, mullite particles, forsterite particles, etc. made of compounds of alumina and/or magnesia may be included.
- organic binders examples include methylcellulose, ethylcellulose, ethylmethylcellulose, carboxymethylcellulose, hydroxypropylmethylcellulose, hydroxyethylcellulose, hydroxymethylcellulose, and hydroxyethylethylcellulose. Among these, it is preferable to use hydroxypropylmethylcellulose and/or methylcellulose.
- the organic binder is preferably contained in an amount of 5 to 15% by mass with respect to 100% by mass of the forming raw material (total of silicon carbide particles and binder).
- water is added to the mixed raw materials and kneaded to form a plastic clay.
- the content of water is adjusted so as to provide a moldable clay hardness, and is preferably 20 to 50% by mass based on the forming raw material.
- the formed clay is extruded from a known honeycomb structure forming mold by a known extrusion method to form a honeycomb structure formed body. After drying the formed body, the end face, outer circumference, etc. are processed as necessary, and the body is fired in an oxidizing atmosphere at a temperature range of 1200 to 1350° C. to produce a silicon carbide ceramic honeycomb structure.
- the drying method is not particularly limited, but examples include hot air drying, microwave heating drying, and high frequency heating drying.
- the alumina source particles and magnesia source particles are sintered to form a bonding layer that bonds the silicon carbide particles together. Since sintering can be performed at a relatively low sintering temperature in this way, the sintering cost for forming the bonding layer can be kept lower than before. If the sintering temperature is less than 1200° C., the bonding between the silicon carbide particles and the binder phase is insufficient, and sufficient strength cannot be obtained. On the other hand, if the temperature exceeds 1350°C, the thermal shock resistance is lowered.
- the firing temperature can be lowered, there is no need to perform firing in a non-oxidizing atmosphere for suppressing oxidation as in the conventional technology, and firing can be performed in an oxidizing atmosphere, so an increase in cost in the firing process can be suppressed.
- Examples 1-10, Comparative Examples 2 and 3 Silicon carbide particles having particle diameters shown in Table 1 and binder particles (alumina source particles and magnesia source particles) were blended and mixed together with hydroxypropylmethyl cellulose as an organic binder in the amounts shown in Table 1 to be added. Water is added to the mixed raw materials and kneaded to form a plastic clay. A molded body with a honeycomb structure having a length of 304 mm was molded. After drying this compact in a hot air dryer at 120°C for 2 hours, it was fired in an oxidizing atmosphere at a maximum temperature of 1300°C to obtain a partition wall thickness of 8 mil (0.20 mm) and a cell density of 300 cpsi (46.5 cells/cm 2 ). ), silicon carbide ceramic honeycomb structures of Examples 1 to 10 and Comparative Examples 2 and 3 were obtained.
- binder particles alumina source particles and magnesia source particles
- Comparative example 1 The types and amounts of silicon carbide particles and binder particles were changed as shown in Table 1, and after the compact was dried with hot air, a degreasing process was added at 550°C for 3 hours, followed by argon at a maximum temperature of 1450°C. A silicon carbide ceramic honeycomb structure of Comparative Example 1 was obtained in the same manner as in Example 1, except that it was fired in the atmosphere for 2 hours.
- Porosity and median pore diameter were measured by a mercury intrusion method.
- a test piece (10 mm ⁇ 10 mm ⁇ 10 mm) cut from a ceramic honeycomb structure was placed in a measurement cell of Autopore III manufactured by Micromeritics. The relationship between the pressure during pressing and the volume of mercury forced into the pores existing in the test piece was obtained. The pressure is converted to a pore diameter, and the cumulative pore volume (corresponding to the volume of mercury) integrated from the larger pore diameter side to the smaller pore diameter side is plotted against the pore diameter, and the pore diameter and the cumulative pore volume are plotted.
- the total pore volume and the median pore diameter which is the pore diameter at which the cumulative pore volume is 50% of the total pore volume, were determined.
- A-axis compressive fracture strength is measured from a ceramic honeycomb structure with a diameter of 24.5 mm in accordance with the standard M505-87 "Testing method for ceramic monolith carriers for automotive exhaust gas purification catalysts" established by the Society of Automotive Engineers of Japan. And a sample piece with a length of 24.5 mm was taken.
- Cordierite (molar ratio M1) cordierite (mol) / [cordierite (mol) + spinel (mol)]
- Spinel (molar ratio) spinel (mol) / [cordierite (mol) + spinel (mol)]
- the ceramic honeycomb filters of Examples 1 to 10 of the present invention had heat resistance equal to or higher than that of the ceramic honeycomb filters of Comparative Examples 1 to 3. It can be seen that it was possible to manufacture at low cost because it was possible to bake at a low maximum temperature without the need for
Abstract
Description
本発明の炭化珪素質セラミックハニカム構造体は、炭化珪素質多孔質体の隔壁により仕切られた軸方向に貫通する多数の流路を有し、前記隔壁が、骨材となる炭化珪素粒子と、前記炭化珪素粒子を結合する結合層とを有し、前記結合層が、少なくともコーディエライト相とスピネル相とを含み、前記コーディエライト相のモル比M1[=コーディエライト相/(コーディエライト相+スピネル相)]が0.4~0.9である。
本発明の炭化珪素質セラミックハニカム構造体の製造方法について、その一実施形態を説明する。
Al(OH)3=(1/2)Al2O3+(3/2)H2O、及び
Mg(OH)2=MgO+H2O
と表されるので、酸化アルミニウム1モルあたりのアルミナ分は0.5モル、酸化マグネシウム1モル中のマグネシア分は1モルと計算できる。この関係から、前述したようにアルミナ分及びマグネシア分のモル数を求め、モル比M2を求める。またアルミナ及びマグネシアの両方を含む化合物(例えば、スピネル)の粒子を用いた場合も同様に、この化合物中のアルミナ分(Al2O3)及びマグネシア分(MgO)を算出してモル比M2を求める。
表1に示す粒径を有する炭化珪素粒子、及び結合材の粒子(アルミナ源粒子及びマグネシア源粒子)を表1に示す添加量で有機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とともに配合し混合した。混合した原料に水を添加して混練して可塑性の坏土を形成し、得られた坏土をハニカム構造体成形用の金型からスクリュー成形機により押出して、一辺が34 mmの外形四角形柱状で長さ304 mmのハニカム構造の成形体を成形した。この成形体を熱風乾燥機にて120℃で2時間乾燥後、1300℃の最高温度で酸化雰囲気で焼成して、隔壁厚さ8 mil(0.20 mm)及びセル密度300 cpsi(46.5セル/cm2)を有する実施例1~10、比較例2及び3の炭化珪素質セラミックハニカム構造体を得た。
炭化珪素粒子及び結合材の粒子の種類及び添加量を表1に示すように変更し、さらに成形体を熱風乾燥した後に550℃で3時間の脱脂工程を追加し、1450℃の最高温度でアルゴン雰囲気で2時間焼成した以外は実施例1と同様にして、比較例1の炭化珪素質セラミックハニカム構造体を得た。
気孔率、及びメジアン細孔径は、水銀圧入法により測定を行った。セラミックハニカム構造体から切り出した試験片(10 mm×10 mm×10 mm)を、Micromeritics社製オートポアIIIの測定セル内に収納し、セル内を減圧した後、水銀を導入して加圧し、加圧時の圧力と試験片内に存在する細孔中に押し込まれた水銀の体積との関係を求めた。前記圧力を細孔径に換算し、細孔径の大きい側から小さい側に向かって積算した累積細孔容積(水銀の体積に相当)を細孔径に対してプロットし、細孔径と累積細孔容積との関係を示すグラフを得た。水銀を導入する圧力は0.5psi(0.35×10-3 kg/mm2)とし、圧力から細孔径を算出する際の常数は、接触角=130°及び表面張力=484 dyne/cmの値を使用した。なお水銀の加圧力が1800psi(1.26kg/mm2、細孔径約0.1μmに相当)での累積細孔容積を全細孔容積とした。
熱膨張係数は、4.5 mm×4.5 mmの断面形状及び50 mmの長さの試験片を、長手方向が流路方向にほぼ一致するように切り出し、熱機械分析装置(TMA、リガク社製ThermoPlus、圧縮荷重方式/示差膨張方式)を用いて、一定荷重20 gをかけながら、昇温速度10℃/minで室温から800℃まで加熱した時の全長方向の長さの増加量を測定して、40~800℃間の平均熱膨張係数として求めた。
A軸圧縮破壊強度は、社団法人自動車技術会が定める規格M505-87「自動車排気ガス浄化触媒用セラミックモノリス担体の試験方法」に従い、セラミックハニカム構造体から直径24.5 mm及び長さ24.5 mmの試料片を採取して行った。
注(2):スピネル(モル比)=スピネル(モル)/[コーディエライト(モル)+スピネル(モル)]
Claims (7)
- 炭化珪素質多孔質体の隔壁により仕切られた軸方向に貫通する多数の流路を有する炭化珪素質セラミックハニカム構造体であって、前記隔壁が、骨材となる炭化珪素粒子と、前記炭化珪素粒子を結合する結合層とを有し、前記結合層が、少なくともコーディエライト相とスピネル相とを含み、前記コーディエライト相のモル比M1[=コーディエライト相/(コーディエライト相+スピネル相)]が0.4~0.9であることを特徴とする炭化珪素質セラミックハニカム構造体。
- 前記隔壁の気孔率が35~50%であることを特徴とする請求項1に記載の炭化珪素質セラミックハニカム構造体。
- 前記隔壁のメジアン細孔径が5~20μmであることを特徴とする請求項1又は2に記載の炭化珪素質セラミックハニカム構造体。
- 炭化珪素粒子と、アルミナ源粒子及びマグネシア源粒子を含む結合材と、有機バインダーとを配合し、混合、及び混練して得られた坏土をハニカム形状に押出成形し、得られた成形体を乾燥後、1200~1350℃の温度範囲で、大気雰囲気下で焼成することを特徴とする請求項1~3に記載の炭化珪素質セラミックハニカム構造体を製造する方法。
- 前記アルミナ源粒子及び前記マグネシア源粒子を、モル比M2[=(Al2O3)/(Al2O3+ MgO)]0.32~0.50で配合することを特徴とする請求項4に記載の炭化珪素質セラミックハニカム構造体の製造方法。
- 前記炭化珪素粒子100質量%に対して、前記アルミナ源粒子及び前記マグネシア源粒子を合計で6~15質量%配合することを特徴とする請求項4又は5に記載の炭化珪素質セラミックハニカム構造体の製造方法。
- 前記結合材のアルミナ源粒子がアルミナ粒子又は水酸化アルミニウム粒子であり、マグネシア源粒子が酸化マグネシウム粒子又は水酸化マグネシウム粒子であることを特徴とする請求項4~6のいずれかに記載の炭化珪素質セラミックハニカム構造体の製造方法。
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