WO2022202910A1 - 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
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- WO2022202910A1 WO2022202910A1 PCT/JP2022/013577 JP2022013577W WO2022202910A1 WO 2022202910 A1 WO2022202910 A1 WO 2022202910A1 JP 2022013577 W JP2022013577 W JP 2022013577W WO 2022202910 A1 WO2022202910 A1 WO 2022202910A1
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- pore
- silicon carbide
- volume
- honeycomb structure
- ceramic honeycomb
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- 239000000919 ceramic Substances 0.000 title claims abstract description 78
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 53
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000011148 porous material Substances 0.000 claims abstract description 195
- 238000005192 partition Methods 0.000 claims abstract description 76
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 143
- 230000001186 cumulative effect Effects 0.000 claims description 40
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 25
- 229910052753 mercury Inorganic materials 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- 239000011230 binding agent Substances 0.000 claims description 21
- 238000009826 distribution Methods 0.000 claims description 10
- 239000004927 clay Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000002459 porosimetry Methods 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 16
- 239000002105 nanoparticle Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 238000005259 measurement Methods 0.000 description 8
- 230000002093 peripheral effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 7
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
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- 230000001590 oxidative effect Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
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- 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
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- 229910000505 Al2TiO5 Inorganic materials 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
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon 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
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- 230000006835 compression Effects 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 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 description 1
- 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 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000001761 ethyl methyl cellulose Substances 0.000 description 1
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- 238000001125 extrusion Methods 0.000 description 1
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- 229920013819 hydroxyethyl ethylcellulose Polymers 0.000 description 1
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- 238000004898 kneading Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000003825 pressing Methods 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
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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Definitions
- the present invention relates to a silicon carbide ceramic honeycomb structure used in a ceramic honeycomb filter and a method for manufacturing the silicon carbide ceramic honeycomb structure.
- 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 including porous partition walls 12 and an outer peripheral wall 11 forming a plurality of outflow-side plugged channels 13 and inflow-side plugged channels 14, channels 13, It consists of an inflow-side sealing portion 16a and an outflow-side sealing portion 16b that alternately seal the exhaust gas inflow-side end face 15a and the outflow-side end face 15b of 14 in a checkered pattern. As indicated by the dotted arrow in FIG. 1(b), the exhaust gas flows from the outflow-side sealed channel 13 opening at the exhaust-gas inflow-side end face 15a, and flows through the thin lines formed on the surface and inside of the partition wall 12.
- Patent Document 1 describes a honeycomb structure capable of capturing even nano-sized fine particles, which comprises a ceramic powder and a binder that binds the ceramic particles that make up the ceramic powder.
- the distance between the 10% particle size (D10) and the 90% particle size (D90) is 10 ⁇ m or more
- the 20% particle size (D20) and the 80% particle size (D80) are logD20 /logD80 ⁇ 0.85 and having two or more peaks when the particle size distribution is measured.
- a binder such as colloidal silica.
- Patent Document 2 Japanese Patent Application Laid-Open No. 2018-149510 (Patent Document 2) describes a plugged honeycomb structure that is excellent in collection performance and capable of suppressing variations in pressure loss.
- a columnar honeycomb structure portion having porous partition walls arranged to surround a plurality of cells serving as channels, and a plugging portion provided in an opening portion of each cell on the inflow end face side or the outflow end face side.
- the pore diameter at which the cumulative pore volume is 10% is D10
- the pore diameter at which the cumulative pore volume is 30% is D30
- the cumulative pore volume is
- D50 is the pore diameter at 50%
- D70 is the pore diameter at which the cumulative pore volume is 70%
- D90 is the pore diameter at which the cumulative pore volume is 90%
- the pore diameter D10 is 6 ⁇ m or more
- Honeycomb structures made with metallic silica powder are described.
- Patent Document 3 discloses a honeycomb structure capable of suppressing an increase in pressure loss even after a catalyst is supported on partition walls, and a fluid flow path extending from a first end surface to a second end surface.
- a columnar honeycomb structure having porous partition walls arranged to surround a plurality of cells, wherein the partition walls have a porosity of 45 to 65% and the partition walls have an average pore diameter of 15 to 25 ⁇ m
- the pore volume ratio of pores with a pore diameter of 10 ⁇ m or less is 10% or less of the total pore volume of the partition walls, and the pore diameter is 40 ⁇ m or more.
- the honeycomb structure has a pore volume ratio of 10% or less, and the partition walls of the honeycomb structure are made of silicon carbide, cordierite, silicon-silicon carbide composite material, cordierite-silicon carbide composite material, silicon nitride , mullite, alumina, and aluminum titanate.
- Patent Document 4 discloses a honeycomb structure capable of improving collection performance, which is arranged so as to surround a plurality of cells serving as fluid flow paths extending from a first end surface to a second end surface. a columnar honeycomb structure portion having porous partition walls; and plugging portions provided in openings of each cell on the first end face side or the second end face side, wherein the partition walls contain silicon carbide.
- the partition wall porosity measured by mercury porosimetry is 42 to 52%, the thickness of the partition walls is 0.15 to 0.36 mm, and the cumulative pore volume of the partition walls measured by mercury porosimetry , the ratio of pore volume with a pore diameter of 10 ⁇ m or less to the total pore volume of the partition walls is 41% or less, and the ratio of pore volume with a pore diameter of 18 to 36 ⁇ m to the total pore volume is 10% or less.
- the pore size at which the log differential pore volume is the maximum value is in the range of 10 to 16 ⁇ m
- the log differential pore It discloses a plugged honeycomb structure in which the half-value width of a peak including the maximum value of volume is 5 ⁇ m or less.
- an object of the present invention is to maintain thermal shock resistance, have a PM collection rate that effectively collects nano-sized PM that greatly affects the number of PM particles, and reduce pressure loss after PM collection.
- An object of the present invention is to provide a good silicon carbide ceramic honeycomb structure and a method for manufacturing the same.
- the present inventors have focused on the morphology of the pores in the cross section of the partition walls of the ceramic honeycomb structure, and as a result, found that the partition walls of the honeycomb structure having a specific pore structure can achieve the above objects. and arrived at the present invention.
- the silicon carbide ceramic honeycomb structure of the present invention has a plurality of flow paths penetrating in the axial direction partitioned by partition walls of the silicon carbide porous body, and the partition walls have a porosity of 35 to 50%.
- the median pore diameter is 8 to 18 ⁇ m, and in the cross section of the partition wall orthogonal to the axial direction, a straight line C passing through the center of the thickness T direction of the partition wall and parallel to the surface of the partition wall, and a straight line C from the straight line C to the partition wall Draw a straight line parallel to the straight line C drawn at ⁇ T / 5 and ⁇ 2T / 5 apart in the thickness direction, and measure the length of the pore portion (pore width) and the number of pores
- the average pore width W which is the average value of the pore widths of all the pores measured, is 10 to 25 ⁇ m, and the unit length, which is the value obtained by dividing the total number of pores measured by the total length of each straight line measured It is
- the relationship between the pore diameter of the partition walls and the cumulative pore volume measured by the mercury intrusion method shows that the pore volume of the partition walls having a pore diameter of 20 ⁇ m or more is the total pore volume. Preferably 10-20% of the volume.
- the relationship between the pore diameter of the partition walls and the cumulative pore volume measured by the mercury intrusion method shows that the pore volume of the pore diameters of 9 ⁇ m or less of the partition walls is the total pore volume. preferably 3 to 25% of the
- ceramic particles containing an aggregate and a binder and an organic binder are blended, mixed and kneaded, and the resulting clay is formed into a honeycomb shape.
- the aggregate is silicon carbide particles
- the ceramic particles are Median particle size D50 is 35-45 ⁇ m
- Particle diameter D10 at the cumulative particle volume equivalent to 10% of the total particle volume is 5 to 20 ⁇ m
- Particle diameter D90 at the cumulative particle volume equivalent to 90% of the total particle volume is 50 to 65 ⁇ m
- the binder is at least one selected from the group consisting of alumina particles, aluminum hydroxide particles, magnesium oxide particles and magnesium hydroxide particles. preferable.
- a ceramic honeycomb can effectively trap nano-sized PM, which greatly affects the number of particles in exhaust gas, while maintaining thermal shock resistance, and has good pressure loss after PM trapping.
- a structure can be provided.
- FIG. 1 is a front view schematically showing an example of a ceramic honeycomb filter
- FIG. 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
- FIG. 4 is a photograph obtained by binarizing a partition wall cross-sectional SEM photograph of the silicon carbide ceramic honeycomb structure of Example 2.
- FIG. It is a schematic diagram for demonstrating the position which measures average pore width and the number of pores per unit length in a partition wall cross section.
- 1 is a graph showing the particle size distribution of ceramic particles used in Examples of the present invention.
- Silicon carbide ceramic honeycomb structure has a plurality of flow paths penetrating in the axial direction partitioned by partition walls of a silicon carbide porous body.
- the partition wall has a porosity of 35 to 50% and a median pore diameter of 8 to 18 ⁇ m, and in a cross section of the partition wall orthogonal to the axial direction, a straight line C passing through the center of the thickness T direction of the partition wall and parallel to the surface of the partition wall.
- the average pore width W which is the average value of the pore widths of all the pores measured, is 10 to 25 ⁇ m
- the total length of each straight line that measures the total number of pores measured The number of pores N per unit length, which is the value divided by , is 20 to 40/mm.
- the ceramic honeycomb structure having such a configuration can effectively trap nano-sized PM while maintaining thermal shock resistance, and the ceramic honeycomb structure has good pressure loss after PM trapping. body can be provided.
- the average pore width W which is the average value of the pore widths measured in the cross section of the partition wall, is 10-25 ⁇ m.
- the lower limit of the average pore width W is preferably 12 ⁇ m, and the upper limit is preferably 23 ⁇ m, more preferably 19 ⁇ m.
- the number of pores N per unit length measured in the cross section of the partition is 20 to 40/mm. If the number of pores N per unit length is less than 20/mm, it becomes difficult to maintain a low pressure loss after collecting PM. On the other hand, if it exceeds 40/mm, the nano-sized PM collection rate is lowered.
- the lower limit of the number of pores N per unit length is preferably 22/mm, and the upper limit is preferably 37/mm.
- the average pore width W and the number of pores per unit length N are obtained by scanning electron microscopy (SEM) of the cross section of the partition wall in the cross section perpendicular to the axial direction of the ceramic honeycomb structure. is obtained as follows using image analysis software (Media Cybernetics Image-Pro Plus ver.7.0). First, the obtained SEM photograph is subjected to black-and-white binarization processing.
- FIG. 4 shows an example of an image subjected to black-and-white binarization processing. Next, as shown in FIG.
- the porosity is 35-50%. If the porosity is less than 35%, it becomes difficult to maintain a low pressure loss after collecting PM. On the other hand, if it exceeds 50%, the nano-sized PM trapping rate decreases.
- the lower limit of porosity is preferably 38%, more preferably 40%.
- the upper limit of porosity is preferably 49%, more preferably 48%, most preferably 46%.
- the porosity of the partition walls is measured by a mercury intrusion method, which will be described later.
- the median pore size is 8-18 ⁇ m. If the median pore size is less than 8 ⁇ m, it becomes difficult to maintain a low pressure loss after collecting PM. On the other hand, when it exceeds 18 ⁇ m, the nano-sized PM trapping rate is lowered.
- the median pore size is preferably 10-15 ⁇ m.
- the median pore diameter is the pore diameter at which the cumulative pore volume is 50% of the total pore volume in the pore distribution curve of partition walls measured by the mercury intrusion method described below.
- the pore volume with a pore diameter of 20 ⁇ m or more is preferably 10-20% of the total pore volume. If the pore volume of 20 ⁇ m or more is less than 10% of the total pore volume, it may be difficult to maintain a low pressure drop after collecting PM. On the other hand, if it exceeds 20%, the capture rate of nano-sized PM may decrease. Preferably, it is 12-18%.
- the pore volume with a pore diameter of 9 ⁇ m or less is preferably 3 to 25% of the total pore volume. If the pore volume with a pore diameter of 9 ⁇ m or less is less than 3% of the total pore volume, it may be difficult to maintain a low pressure loss after PM collection. On the other hand, if it exceeds 25%, the capture rate of nano-sized PM may decrease.
- the lower limit is preferably 4% and the upper limit is preferably 23%.
- Measurement of cumulative pore volume by mercury porosimetry is performed using, for example, Autopore III 9410 manufactured by Micromeritics.
- the cumulative pore volume was measured by the mercury intrusion method.
- a test piece (10 mm ⁇ 10 mm ⁇ 10 mm) cut from a ceramic honeycomb structure was placed in a measurement cell, the pressure inside the cell was reduced, and then mercury was introduced. This is done by determining the volume of mercury forced into the pores present in the specimen when the specimen is pressurized with At this time, as the pressure increases, mercury penetrates into finer pores. It is possible to obtain the relationship between the accumulated pore volume from the pore diameter of 1 to the specific pore diameter).
- Mercury permeates sequentially from the larger pore diameter to the smaller pore diameter, and the pressure is converted to the pore diameter, and the cumulative pore volume (equivalent to the volume of mercury) integrated from the larger pore diameter side to the smaller pore diameter side ) is plotted against the pore size.
- the pressure for introducing mercury is 0.5 psi (0.35 ⁇ 10 ⁇ 3 kg/mm 2 , equivalent to a pore diameter of about 362 ⁇ m), and the pressure of mercury is 1800 psi (1.26 kg/mm 2 , a pore diameter of about 0.1 ⁇ m equivalent to ) is the total pore volume.
- 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.
- a coating material is applied to the subsequent outer peripheral surface to form the outer peripheral wall 21 .
- the exhaust gas inlet side 25a or the exhaust gas outlet side 25b of the flow path is plugged alternately in a checkered pattern by a known method to form the ceramic honeycomb filters 100, 200.
- the sealing portions 26a and 26b may be formed in the honeycomb segments 211 before being joined, or the sealing portions 26a may be formed after joining and integrating. , 26b may be formed.
- these sealing portions may be formed on the end surface portion of the exhaust gas inflow side or the exhaust gas outflow side of the flow path, or may be formed at a position inside the flow path from the inflow side end surface 25a or the outflow side end surface 26b. may be formed in
- the particle diameter D10 at the cumulative particle volume is 5-20 ⁇ m
- the particle diameter D90 at the cumulative particle volume equivalent to 90% of the total particle volume is 50-65 ⁇ m
- the particle size distribution deviation SD log(D80)-log (D20), where D20 is the particle diameter at the cumulative particle volume equivalent to 20% of the total particle volume, D80 is the particle diameter at the cumulative particle volume equivalent to 80% of the total particle volume, and D20 ⁇ D80 ] is between 0.20 and 0.40.
- the porosity of the partition walls is 35 to 50%
- the median pore diameter is 8 to 18 ⁇ m
- the average pore width W is 10 to 25 ⁇ m and per unit length in the partition wall cross section orthogonal to the axial direction.
- a silicon carbide ceramic honeycomb structure having a number of pores N of 20 to 40/mm can be obtained.
- the particle size of the ceramic particles can be measured, for example, using a Microtrac particle size distribution analyzer (MT3000) manufactured by Nikkiso Co., Ltd.
- FIG. 6 shows an example of the relationship between the measured particle diameter and the cumulative particle volume (a value obtained by accumulating the volume of particles with a specific particle diameter or less).
- D10 ( ⁇ m) is the particle diameter at the cumulative particle volume equivalent to 10% of the total particle volume
- D50 ( ⁇ m) the median particle diameter
- D90 ( ⁇ m) is the particle diameter at the cumulative particle volume corresponding to 90% of the total particle volume.
- the ceramic particles have a median particle diameter D50 of 35 to 45 ⁇ m.
- D50 median particle size
- the lower limit of the median particle size D50 is preferably 37 ⁇ m, and the upper limit is preferably 43 ⁇ m.
- the D10 of the ceramic particles is 5-20 ⁇ m. If D10 is less than 5 ⁇ m, the ratio of micropores that deteriorate the pressure loss characteristics increases among the pores formed in the partition walls, which is not preferable. On the other hand, if it exceeds 20 ⁇ m, it may be difficult to effectively collect nano-sized PM.
- the lower limit of D10 is preferably 7 ⁇ m and the upper limit is preferably 18 ⁇ m.
- the D90 of ceramic particles is 50-65 ⁇ m.
- D90 is less than 50 ⁇ m, it becomes difficult to maintain low pressure loss when PM is trapped.
- the nano-sized PM trapping rate is lowered.
- the lower limit of D90 is preferably 52 ⁇ m and the upper limit is 63 ⁇ m.
- SD log(D80) - log(D20), where D20 is the particle diameter in the cumulative particle volume equivalent to 20% of the total particle volume, D80 is the 80% of the total particle volume. % and D20 ⁇ D80] is 0.20 to 0.40. If the SD is less than 0.20, the ratio of micropores among the pores formed in the partition walls increases, making it difficult to maintain a low pressure drop when PM is trapped. On the other hand, if it exceeds 0.40, the ratio of coarse pores, which lowers the capture rate of nano-sized PM, increases, which is not preferable.
- the lower limit of SD is preferably 0.22 and the upper limit is preferably 0.38.
- the binder is preferably at least one selected from the group consisting of alumina particles, aluminum hydroxide particles, magnesium oxide particles, and magnesium hydroxide particles.
- 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).
- a plastic clay is formed by blending ceramic particles containing aggregates and binders with an organic binder, adding water to the mixed raw materials, and kneading them.
- 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.
- binder particles at least one selected from the group consisting of alumina particles, aluminum hydroxide particles, magnesium oxide particles, and magnesium hydroxide particles
- sintering can be performed at a relatively low sintering temperature in this manner, the sintering cost for forming the bonding layer can be kept lower than in the conventional art. If the temperature is less than 1200° C., the bonding between the silicon carbide particles and the binder phase becomes insufficient and sufficient strength cannot be obtained. On the other hand, if the temperature exceeds 1350°C, the thermal shock resistance is lowered. Moreover, since the firing is performed in an oxidizing atmosphere, an increase in cost in the firing process can be suppressed.
- Examples 1-5 Silicon carbide particles having particle diameters shown in Table 1 and particles other than silicon carbide in the amounts shown in Table 1 were blended and mixed together with hydroxypropylmethyl cellulose as an organic binder. Water is added to the mixed raw materials and kneaded to form a plastic clay, which is extruded from a mold for forming a honeycomb structure using a screw forming machine to obtain a square outer shape with a side of 34 mm and a length. A 304 mm honeycomb structure molded body was molded.
- Comparative Examples 1 and 7 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. Silicon carbide ceramic honeycomb structures of Comparative Examples 1 and 7 were obtained in the same manner as in Example 1, except that they were fired in the atmosphere for 2 hours.
- Comparative Examples 2-6 The types and amounts of the silicon carbide particles and binder particles were changed as shown in Table 1, and honeycomb structure molded bodies were formed in the same manner as in Example 1. Silicon carbide ceramic honeycomb structures of Comparative Examples 2 to 6 were obtained in the same manner as in Example 1, except that in Comparative Example 3 the firing was performed at a maximum temperature of 1400° C. in an oxidizing atmosphere.
- Average pore width and number of pores per unit length are measured as follows. A cross section of the partition walls in a cross section perpendicular to the axial direction of the ceramic honeycomb structure is imaged with a scanning electron microscope (SEM) at a magnification of 200 times. The captured SEM photograph is measured with image analysis software (Image-Pro Plus ver.7.0 manufactured by Media Cybernetics). Specifically, the captured SEM photograph is subjected to black-and-white binarization processing shown in FIG. 4 using image analysis software. Then, as shown in FIG.
- 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.
- plugging material slurries made of silicon carbide particles were applied so as to alternately plug the channel ends of the silicon carbide ceramic honeycomb structures of Examples 1 to 5 and Comparative Examples 1 to 7. After filling, the plugging material slurry was dried to form a sealed portion.
- a silicon carbide ceramic honeycomb structure in which a sealing portion is formed is used as a honeycomb segment, a bonding material composed of silicon carbide particles and colloidal silica is applied to the outer peripheral surface of the honeycomb segment, and 6 pieces ⁇ 6 layers are joined and integrated, The outer peripheral portion was removed so that the outer peripheral shape of the cross section perpendicular to the axial direction was circular.
- the removed outer periphery is coated with a skin material made of amorphous silica and colloidal silica and dried to form an outer peripheral wall.
- Bonded silicon carbide ceramic honeycomb filters of Examples 1-5 and Comparative Examples 1-7 having a cell density of 300 cpsi (46.5 cells/cm 2 ) were obtained. Two identical ceramic honeycomb filters were manufactured.
- the pressure loss is (x) when exceeding 2.8 kPa, ( ⁇ ) when exceeding 2.5 kPa and 2.8 kPa or less, ( ⁇ ) when exceeding 2.3 kPa and 2.5 kPa or less, and 2.3 kPa or less ( ⁇ ) was evaluated as the pressure loss after PM collection.
- PM collection rate based on the number of particles after collection Then, while feeding combustion soot with an average particle size of 0.11 ⁇ m at a rate of 1.3 g/h, the number of combustion soot particles flowing into the honeycomb filter and the number of combustion soot particles flowing out of the honeycomb filter per minute were counted by SMPS. (Scanning Mobility Particle Sizer) (TIS model 3936), the number of particles Nin of combustion soot flowing into the honeycomb filter and outflowing from the honeycomb filter in 1 minute from 40 minutes to 41 minutes after the start of feeding The PM collection rate was obtained from the number of particles Nout of the combusted soot by the formula: (Nin-Nout)/Nin. PM collection rate is 98% or more ( ⁇ ), ( ⁇ ) when 96% or more and less than 98% ( ⁇ ) when 95% or more and less than 96%, and If less than 95% ( ⁇ ) was evaluated as the PM collection rate after PM collection.
- the ceramic honeycomb filters of Examples 1 to 5 whose porosity, median pore diameter, average pore width in the cross section of partition walls, and number of pores are within the scope of the present invention, meet these requirements. Compared to the ceramic honeycomb filters of Comparative Examples 1 to 7, which are out of the range of It turns out that it is good.
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Abstract
Description
前記骨材が炭化珪素粒子であり、
前記セラミックス粒子は、
メジアン粒子径D50が35~45μm、
粒子径と累積粒子体積との関係を示す曲線において、
全粒子体積の10%に相当する累積粒子体積での粒子径D10が5~20μm、
全粒子体積の90%に相当する累積粒子体積での粒子径D90が50~65μm、
粒度分布偏差SD[ただし、SD=log(D80)-log(D20)であり、D20は全粒子体積の20%に相当する累積粒子体積での粒子径、D80は全粒子体積の80%に相当する累積粒子体積での粒子径でありD20<D80である]が0.20~0.40であることを特徴とする。
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複数の流路を有し、前記隔壁の気孔率が35~50%、メジアン細孔径が8~18μmであり、前記軸方向に直交する前記隔壁の断面において、前記隔壁の厚さT方向の中心を通り前記隔壁の表面に平行な直線C、並びに前記直線Cから前記隔壁の厚さ方向に±T/5及び±2T/5離れた位置に引いた直線Cに平行な直線を引き、各直線が横切る気孔部分の長さ(気孔幅)及び気孔の数を所定の長さについて測定したとき、測定した全ての気孔の気孔幅の平均値である平均気孔幅Wが10~25μm、及び測定した気孔の総数を測定した各直線の全長さで割った値である単位長さ当たりの気孔数Nが20~40個/mm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。
骨材と結合材とを含むセラミックス粒子と、有機バインダーとを配合し、混合、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、焼成して製造する。ここで、前記骨材が炭化珪素粒子であり、前記セラミックス粒子は、メジアン粒子径D50が35~45μm、粒子径と累積粒子体積との関係を示す曲線において、全粒子体積の10%に相当する累積粒子体積での粒子径D10が5~20μm、全粒子体積の90%に相当する累積粒子体積での粒子径D90が50~65μm、粒度分布偏差SD[ただし、SD=log(D80)-log(D20)であり、D20は全粒子体積の20%に相当する累積粒子体積での粒子径、D80は全粒子体積の80%に相当する累積粒子体積での粒子径でありD20<D80である]が0.20~0.40である。
表1に示す粒径を有する炭化珪素粒子、炭化珪素以外の粒子を表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、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成形して、一辺が34 mmの外形四角形状で長さ304 mmのハニカム構造成形体を成形した。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1~5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及び7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て、実施例1と同様にハニカム構造成形体を成形し、比較例2及び4~6は1300℃の最高温度で、比較例3は1400℃の最高温度で酸化雰囲気で焼成した以外は実施例1と同様にして、比較例2~6の炭化珪素質セラミックハニカム構造体を得た。
平均気孔幅、及び単位長さ当たりの気孔数は、次のように測定する。
セラミックスハニカム構造体の軸方向に直交する断面における隔壁の断面を走査型電子顕微鏡(SEM)で倍率200倍で撮像する。撮像されたSEM写真を画像解析ソフト(Media Cybernetics 社製 Image-Pro Plus ver.7.0)で測定する。具体的には、撮像されたSEM写真を画像解析ソフトで図4に示す白黒2値化処理を行う。そして、図5に示すように、撮像された隔壁12の断面において、隔壁の厚さT方向の中心を通り隔壁の表面に平行な直線Cと、この直線Cから隔壁の厚さ方向に±T/5及び±2T/5離れた位置に直線Cに平行な直線を引く。各直線が横切る気孔部分の長さである気孔幅と、各直線が横切る気孔の数とを所定の長さについて測定したとき、測定した全ての気孔幅の合計長さを、測定した気孔の総数で割った値を平均気孔幅Wとし、測定した気孔の総数を、測定した各直線の全長さで割った値を単位長さ当たりの気孔数Nとした。
気孔率、及びメジアン細孔径は、水銀圧入法により測定した。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0.5 psi(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1800 psi(1.26 kg/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。結果を表2に示す。
PM捕集後の圧力損失は、圧力損失テストスタンドに固定したセラミックハニカムフィルタに、空気流量10 Nm3/minで、平均粒径0.11μmの燃焼煤を1.3 g/hの速度で投入し、フィルタ体積1リットルあたりの煤付着量が2 gとなった時の流入側と流出側との差圧(圧力損失)から以下の基準により評価した。すなわち、圧力損失が、
2.8 kPaを越える場合を(×)、
2.5 kPaを超え2.8 kPa以下の場合を(△)、
2.3 kPaを超え2.5 kPa以下の場合を(○)、及び
2.3 kPa以下の場合を(◎)
としてPM捕集後の圧力損失を評価した。
捕集後の粒子数基準でのPM捕集率は、圧力損失テストスタンドに固定したセラミックハニカムフィルタに、空気流量10 Nm3/minで、平均粒径0.11μmの燃焼煤を1.3 g/hの速度で投入しながら、1分毎にハニカムフィルタに流入する燃焼煤の粒子数とハニカムフィルタから流出する燃焼煤の粒子数とをSMPS(Scanning Mobility Particle Sizer)(TIS社製モデル3936)を用いて計測し、投入開始40分後から41分後までの1分間にハニカムフィルタに流入する燃焼煤の粒子数Nin、及びハニカムフィルタから流出する燃焼煤の粒子数Noutから、式:(Nin-Nout)/Nin によりPM捕集率を求めた。PM捕集率が、
98%以上の場合を(◎)、
96%以上98%未満の場合を(○)、
95%以上96%未満の場合を(△)、及び
95%未満の場合を(×)
としてPM捕集後のPM捕集率を評価した。
Claims (5)
- 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複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、
前記隔壁の気孔率が35~50%、メジアン細孔径が8~18μmであり、
前記軸方向に直交する前記隔壁の断面において、
前記隔壁の厚さT方向の中心を通り前記隔壁の表面に平行な直線C、並びに前記直線Cから前記隔壁の厚さ方向に±T/5及び±2T/5離れた位置に引いた直線Cに平行な直線を引き、
各直線が横切る気孔部分の長さ(気孔幅)及び気孔の数を所定の長さについて測定したとき、
測定した全ての気孔の気孔幅の平均値である平均気孔幅Wが10~25μm、及び
測定した気孔の総数を測定した各直線の全長さで割った値である単位長さ当たりの気孔数Nが20~40個/mm
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。 - 水銀圧入法によって測定された前記隔壁の細孔径と累積細孔容積との関係において、前記隔壁の細孔径が20μm以上の細孔容積が全細孔容積の10~20%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。
- 水銀圧入法によって測定された前記隔壁の細孔径と累積細孔容積との関係において、前記隔壁の細孔径9μm以下の細孔容積が全細孔容積の3~25%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。
- 骨材と結合材とを含むセラミックス粒子と、有機バインダーとを配合し、混合、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、焼成して請求項1~3のいずれか1項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であって、
前記骨材が炭化珪素粒子であり、
前記セラミックス粒子は、
メジアン粒子径D50が35~45μmであり、
粒子径と累積粒子体積との関係を示す曲線において、
全粒子体積の10%に相当する累積粒子体積での粒子径D10が5~20μm、
全粒子体積の90%に相当する累積粒子体積での粒子径D90が50~65μm、
粒度分布偏差SD[ただし、SD=log(D80)-log(D20)であり、D20は全粒子体積の20%に相当する累積粒子体積での粒子径、D80は全粒子体積の80%に相当する累積粒子体積での粒子径でありD20<D80である]が0.20~0.40
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の製造方法。 - 前記結合材が、アルミナ粒子、水酸化アルミニウム粒子、酸化マグネシウム粒子、水酸化マグネシウム粒子からなる群から選ばれた少なくとも1種であ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。
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