CN117142874A - Thin-wall silicon carbide honeycomb ceramic carrier and preparation method and application thereof - Google Patents
Thin-wall silicon carbide honeycomb ceramic carrier and preparation method and application thereof Download PDFInfo
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- CN117142874A CN117142874A CN202311435728.2A CN202311435728A CN117142874A CN 117142874 A CN117142874 A CN 117142874A CN 202311435728 A CN202311435728 A CN 202311435728A CN 117142874 A CN117142874 A CN 117142874A
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- powder
- silicon carbide
- silicon
- honeycomb ceramic
- thin
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 32
- 239000010703 silicon Substances 0.000 claims abstract description 32
- 239000011230 binding agent Substances 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 19
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 19
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 15
- 239000000314 lubricant Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 11
- 239000011265 semifinished product Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- 238000005238 degreasing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000004080 punching Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000007688 edging Methods 0.000 claims abstract description 4
- 238000004898 kneading Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 238000007493 shaping process Methods 0.000 claims abstract description 4
- 102220043159 rs587780996 Human genes 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 5
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 5
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 5
- 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 claims description 5
- 229920000609 methyl cellulose Polymers 0.000 claims description 5
- 239000001923 methylcellulose Substances 0.000 claims description 5
- 235000010981 methylcellulose Nutrition 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 4
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000002199 base oil Substances 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 241000276425 Xiphophorus maculatus Species 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 13
- 239000011148 porous material Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 238000001125 extrusion Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0006—Honeycomb structures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
- F01N3/2825—Ceramics
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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Abstract
The invention discloses a thin-wall silicon carbide honeycomb ceramic carrier and a preparation method and application thereof, wherein the preparation method comprises the following steps: taking silicon inorganic powder, kaolin powder, a pore-forming agent, a binder and an auxiliary agent, and uniformly mixing the silicon inorganic powder, the kaolin powder, the pore-forming agent, the binder and the auxiliary agent by a dry method to obtain a mixture A, wherein the silicon inorganic powder comprises silicon carbide powder and metal silicon powder; adding water and a lubricant into the mixture A, kneading into mud blocks, and processing into mud sections; extruding the prepared mud section out of the honeycomb structure, and then drying, shaping, cutting, punching and plugging holes to obtain a green body; sequentially degreasing and sintering, atmosphere sintering and oxidizing and sintering the green body to obtain a thinned silicon carbide powder honeycomb ceramic semi-finished product; and splicing, edging and surrounding edge treatment are sequentially carried out on the obtained semi-finished product of the silicon carbide powder honeycomb ceramic to obtain a finished product of the silicon carbide powder honeycomb ceramic. Through adding additives and sheet materials, the interaction among particles is changed, the plasticity and strength of the mud section are improved, and the requirements of the future market on the thinning of the silicon carbide powder ceramic carrier can be met.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to a thin-wall silicon carbide honeycomb ceramic carrier, and a preparation method and application thereof.
Background
The tail gas of motor vehicles contains a large amount of harmful substances including carbon monoxide, nitrogen oxides, hydrocarbon, solid suspended particles and the like. The solid suspended particles have complex components and strong adsorption capacity, and can adsorb various metal dust, benzopyrene which is a strong cancerogenic substance, pathogenic microorganisms and the like. The solid suspended particles enter the lung of the human body along with the respiration and stay at different parts of the respiratory tract in the modes of collision, diffusion, deposition and the like, thereby causing respiratory diseases and even forming malignant tumors. The current effective measure for treating the solid suspended particles in the tail gas of the motor vehicle is to utilize a wall-flow ceramic honeycomb carrier, so that the tail gas passes through the wall surface of the ceramic honeycomb carrier, and the solid suspended particles with large particle size are intercepted in the carrier to prevent the solid suspended particles from flowing into the air. However, with the increasing stringent emission regulations, the requirements on the carrier are increasing, so that thin-walled honeycomb ceramic carriers are becoming increasingly available. The wall thickness of the silicon carbide powder honeycomb carrier meeting the requirements of national six (commercial vehicle) and national four (non-road) regulations is generally 10-12mil, but with the difference and continuous tightening of the regulations of various countries, the back pressure requirement on the wall flow type honeycomb carrier is further reduced in the future, and one effective measure for reducing the back pressure of the honeycomb ceramic carrier is to reduce the wall thickness of the honeycomb carrier, however, the preparation of the thin-wall ceramic honeycomb carrier faces more challenges. The thinning of the wall flow type carrier has finer requirements on the granularity of raw materials, mainly because the honeycomb ceramics are molded in an extrusion mode, the narrower the slot width of a die is, the finer the granularity of the raw materials which are allowed to pass, meanwhile, because the irregular shape of the raw materials is easier to bridge, the plasticity of mud segments is poor, the extrusion molding is difficult, the raw material particles are sufficiently fine, but the median pore diameter and the porosity of the silicon carbide powder honeycomb ceramics are mainly formed by stacking particles, the too fine particles can cause the too low pore diameter and the porosity of the product, the back pressure is increased instead, the granularity refinement of the raw materials is ensured, the sufficient pore diameter and the porosity of the product are ensured, the characteristics of thin wall, pore diameter and porosity are a pair of contradiction points, the thinning of the product is realized, and the strength of the product is reduced, so the problem between the pore diameter, the porosity and the strength of the silicon carbide powder product needs to be thinned.
Disclosure of Invention
In order to solve the technical problems, one of the purposes of the invention is to provide a preparation method for preparing a silicon carbide powder honeycomb ceramic carrier with high strength, 6-8mil wall thickness, 10-15 mu m median pore diameter and 40-45% porosity.
In order to achieve the above object, the technical scheme of the present invention is as follows: a preparation method of a thin-wall silicon carbide honeycomb ceramic carrier comprises the following steps:
step 1: taking silicon inorganic powder, kaolin powder, a pore-forming agent, a binder and an auxiliary agent, and uniformly mixing the silicon inorganic powder, the kaolin powder, the pore-forming agent, the binder and the auxiliary agent by a dry method to obtain a mixture A, wherein the silicon inorganic powder comprises silicon carbide powder and metal silicon powder;
step 2: adding water and a lubricant into the mixture A, kneading into mud blocks, and processing into mud sections;
step 3: extruding the prepared mud section into a honeycomb structure, drying and shaping, and sequentially cutting, punching and plugging to obtain a green body;
step 4: sequentially degreasing and sintering, atmosphere sintering and oxidizing and sintering the green body to obtain a thinned silicon carbide powder honeycomb ceramic semi-finished product;
step 5: and splicing, edging and surrounding edge treatment are sequentially carried out on the obtained semi-finished product of the silicon carbide powder honeycomb ceramic to obtain a finished product of the silicon carbide powder honeycomb ceramic.
According to the technical scheme, the adding amount of the silicon carbide powder in the silicon inorganic powder is less than or equal to 83wt% and the balance is the metal silicon powder, the adding amount of the kaolin powder in the step 1 is less than or equal to 3% of the total weight of the silicon inorganic powder, and the pore-forming agent is less than or equal to 10% of the total weight of the silicon inorganic powder.
In the technical scheme, the granularity D50=24-30 mu m and D100 is less than or equal to 90 mu m of the silicon carbide powder; the granularity D50=6-10 mu m and D100 is less than or equal to 25 mu m of the metal silicon powder; the kaolin powder is of a platy structure, the granularity D50=1-5 mu m and the D100 is less than or equal to 63 mu m; the pore-forming agent has a spherical structure, the granularity D50=20-40 μm and the granularity D100 is less than or equal to 75 μm.
In the above technical scheme, the addition amount of the binder is 9-12% of the total weight of the silicon inorganic powder, and/or the binder is at least one of methylcellulose, hydroxypropyl methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyvinyl alcohol, clay and bentonite.
In the technical scheme, the auxiliary agent is at least one of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent, and/or the addition amount of the auxiliary agent is 1-3% of the total weight of the silicon inorganic powder.
In the above technical scheme, the lubricant in the step 2 is at least one of calcium stearate, white oil, base oil, glycerin, polyethylene glycol, synthetic fatty acid and water-soluble polyamide, and/or the adding amount of the lubricant in the step 2 is 3-5% of the total weight of the silicon inorganic powder.
The conditions of the atmosphere sintering in the step 4 in the technical scheme are as follows: under the protection of argon and reducing gas, the sintering temperature is raised to 1410-1450 ℃ from room temperature for heat preservation for 2-4h.
In the technical scheme, the temperature rising rate is less than 300 ℃ per hour in the process of rising the temperature from room temperature to 800 ℃ during the sintering of the atmosphere, the temperature rising rate is less than 10 ℃ per hour in the process of rising the temperature from 800 ℃ to 1100 ℃, and finally the temperature is raised to the heat preservation temperature at the temperature rising rate of less than 5 ℃ per hour.
The invention also provides a thin-wall silicon carbide honeycomb ceramic carrier prepared by the preparation method.
The invention also provides application of the thin-wall silicon carbide honeycomb ceramic carrier, which can be used as a diesel vehicle particle catcher catalyst carrier.
The invention has the beneficial effects that: according to the embodiment of the invention, through adding additives and sheet materials, the interaction among particles is changed, the plasticity and strength of a mud section are improved, the silicon carbide powder honeycomb ceramic carrier with the wall thickness of 6-8mil, the median pore diameter of 10-15 mu m, the porosity of 40-45%, the A-axis compressive strength of more than 10MPa and the B-axis compressive strength of more than 1MPa is prepared, and the requirements of the market for thinning the silicon carbide powder ceramic carrier in the future can be met.
Drawings
FIG. 1 shows the micropore distribution of a thin-walled silicon carbide ceramic honeycomb carrier prepared in example 6 of the present invention;
FIG. 2 is an SEM micrograph of a thin-walled silicon carbide ceramic honeycomb support prepared according to example 6 of the invention;
FIG. 3 is an SEM micrograph of a thin-walled silicon carbide ceramic honeycomb support prepared according to example 6 of the invention;
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The embodiment of the invention provides a preparation method of a thin-wall silicon carbide honeycomb ceramic carrier, which comprises the following steps:
step 1: taking silicon inorganic powder, kaolin powder, a pore-forming agent, a binder and an auxiliary agent, and uniformly mixing the silicon inorganic powder and the pore-forming agent by a dry method to obtain a mixture A (the silicon inorganic powder comprises silicon carbide powder and metal silicon powder, the addition amount of the silicon carbide powder in the silicon inorganic powder is less than or equal to 83wt%, the balance is the metal silicon powder, the addition amount of the kaolin powder is less than or equal to 3% of the total weight of the silicon inorganic powder, the pore-forming agent is less than or equal to 10% of the total weight of the silicon inorganic powder, the particle size D50=24-30 μm of the silicon carbide powder, D100 is less than or equal to 90 μm, the particle size D50=6-10 μm of the metal silicon powder, D100 is less than or equal to 25 μm, the kaolin powder is of a sheet-like structure, the particle size D50=1-5 μm, D100 is less than or equal to 63 μm, the pore-forming agent is of a spherical structure, the particle size D50=20-40 μm, the addition amount of the binder is less than or equal to 75 μm, the binder is 9-12% of the total weight of the silicon inorganic powder, the binder is methyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl cellulose, polyvinyl alcohol, at least one of the clay and at least one of the coupling agents is 3% of coupling aids;
step 2: adding water and a lubricant into the mixture A and kneading the mixture A into mud blocks (the adding amount of the water is proper and the mixture A and the mud blocks are formed), and processing the mixture A into mud sections by adopting a mud pugging machine (the lubricant is at least one of calcium stearate, white oil, base oil, glycerol, polyethylene glycol, synthetic fatty acid and water-soluble polyamide, and the adding amount of the lubricant in the step 2 is 3-5% of the total weight of the silicon inorganic powder);
step 3: extruding the prepared mud section into a honeycomb structure, drying and shaping (drying by microwaves), and sequentially performing cutting, punching and hole blocking treatment (wherein the cutting, punching and hole blocking technology belongs to the prior art and is not described in detail herein) to obtain a green body;
step 4: sequentially degreasing sintering, atmosphere sintering and oxidizing sintering the green body to obtain a thinned silicon carbide powder honeycomb ceramic semi-finished product (the heating rate is less than 300 ℃/h in the process of heating from room temperature to 800 ℃ in the atmosphere sintering, the heating rate is less than 10 ℃/h in the process of heating from 800 ℃ to 1100 ℃, and finally the heating rate is less than 5 ℃/h to the heat preservation temperature);
step 5: and splicing, edging and surrounding edge treatment are sequentially carried out on the obtained semi-finished product of the silicon carbide powder honeycomb ceramic to obtain a finished product of the silicon carbide powder honeycomb ceramic.
The binder in this embodiment may be further divided into an organic binder and an inorganic binder, wherein the organic binder is at least one of Methylcellulose (MC), hydroxypropyl methylcellulose (HPMC), carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC) and polyvinyl alcohol (PVA), and the inorganic binder is at least one of clay and bentonite.
The raw materials of inorganic raw materials (silicon carbide powder, metal silicon powder, kaolin powder and pore-forming agent) in the thin-wall silicon carbide honeycomb ceramic carrier in the embodiment of the invention are shown in table 1:
table 1: list of raw materials
The components and the detection results of the examples and comparative examples of the present invention are shown in Table 2:
TABLE 2 Components and detection Table for examples 1-7 and comparative examples 1-3
Note that: the unit of each component content in table 2 is% in which the sum of the added amounts of silicon carbide powder and metal silicon powder is the total amount of silicon inorganic powder, and the added amounts of silicon carbide powder, metal silicon powder, kaolin powder, pore-forming agent, organic binder, inorganic binder, auxiliary agent and lubricant are all calculated by the total amount of silicon inorganic powder (taking example 1 as an example, if the total amount of silicon inorganic powder is 100 parts by weight, the added amount of silicon carbide powder is 75 parts, the added amount of metal silicon powder is 25 parts, the added amount of kaolin powder is 0 part, the added amount of pore-forming agent is 9 parts, the added amount of organic binder is 9 parts, the added amount of inorganic binder is 0 part, the added amount of auxiliary agent is 0 part, the added amount of lubricant is 1 part), and "-" in table 2 indicates that no addition, the evaluation criteria of the extrusion evaluation in table 2 are as follows: a: under the same condition, the extrusion rate is more than 70mm/s; b: under the same conditions, the extrusion rate is 40-70mm/s; c: under the same conditions, the extrusion rate is 10-40mm/s; d: under the same conditions, extrusion speedThe rate is less than 10mm/s; wherein, the equivalent condition means: the same equipment has the same mud section hardness, extrusion pressure and screen mesh number (mud section hardness 22 kg/cm) 2 The technical pressure is 10MPa, the mesh number is 100), and the particle sizes D50 and D100 of the inorganic raw materials used in comparative example 1, comparative example 2, and examples 1 to 7 are shown in table 1, wherein the compressive a and compressive B in table 2 respectively represent the compressive strength of a-axis and the compressive strength of B-axis (the a-axis means a direction parallel to the duct and the B-axis means a direction perpendicular to the duct), in MPa, and the pore diameters, D10, and D90 are in μm, and the measurement methods of the respective indexes in the above table 2 in the examples of the present invention are all prior art, and are not described herein.
In comparative example 3, the inorganic raw materials used were the same as the raw material D50 used in example 6, but D100 of each inorganic raw material was out of the range defined in table 1 to prepare a ceramic honeycomb carrier, which had poor mud segment plasticity, and problems of difficult extrusion and broad micropore distribution were likely to occur.
As can be seen from comparative examples 1, 2 and 2-5 (comparative examples 1 and 2), the mud section plasticity is significantly increased by adding the auxiliary agent and kaolin powder, mainly because one side group of the auxiliary agent can physically and chemically react with the surface of the inorganic material, and the other side group can physically and chemically react with the polymer material after adding the auxiliary agent, and the bridge of the auxiliary agent changes the surface state of the powder, and can hinder the bridging effect between the powders, thereby improving the mud section plasticity. The plasticity of the kaolin powder is increased mainly due to the flaky structure, the flaky structure can be filled among irregular particles, and the effects of lubrication and blocking particle bridging can be achieved, so that the plasticity of a mud segment can be increased, and meanwhile, the kaolin powder has certain viscosity and contains Al 2 O 3 Higher amounts can act as part of the binder as well as increase the green degreasing strength.
As can be seen from comparative examples 1, 6 and 7, when the pore-forming agent reaches a certain amount, the median pore diameter tends to decrease, probably due to the fact that the residual carbon content generated by the pore-forming agent during sintering increases, and the residual carbon reacts with part of the metal silicon powder to block the pore channels.
As can be seen from comparative examples 1 to 3 and examples 1 to 7, the thinned silicon carbide powder honeycomb ceramics can be produced by adjusting the ratio of the raw materials, the particle size distribution, the addition of the auxiliary agent and the appropriate pore-forming agent.
From fig. 1, it can be known that the microporous distribution of the silicon carbide powder honeycomb ceramic product corresponding to example 6 is narrow, which is favorable for capturing soot particles, and from fig. 2 and 3, it can be seen that the microporous distribution of the silicon carbide powder honeycomb ceramic product corresponding to example 6 is relatively uniform and the penetrability of the pores is relatively good.
The foregoing has outlined rather broadly the more detailed description of embodiments of the invention, wherein the principles and embodiments of the invention are explained in detail using specific examples, the above examples being provided solely to facilitate the understanding of the method and core concepts of the invention; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present invention, the present description should not be construed as limiting the present invention.
Claims (10)
1. The preparation method of the thin-wall silicon carbide honeycomb ceramic carrier is characterized by comprising the following steps of:
step 1: taking silicon inorganic powder, kaolin powder, a pore-forming agent, a binder and an auxiliary agent, and uniformly mixing the silicon inorganic powder, the kaolin powder, the pore-forming agent, the binder and the auxiliary agent by a dry method to obtain a mixture A, wherein the silicon inorganic powder comprises silicon carbide powder and metal silicon powder;
step 2: adding water and a lubricant into the mixture A, kneading into mud blocks, and processing into mud sections;
step 3: extruding the prepared mud section into a honeycomb structure, drying and shaping, and sequentially cutting, punching and plugging to obtain a green body;
step 4: sequentially degreasing and sintering, atmosphere sintering and oxidizing and sintering the green body to obtain a thinned silicon carbide powder honeycomb ceramic semi-finished product;
step 5: and splicing, edging and surrounding edge treatment are sequentially carried out on the obtained semi-finished product of the silicon carbide powder honeycomb ceramic to obtain a finished product of the silicon carbide powder honeycomb ceramic.
2. The method for preparing the thin-wall silicon carbide honeycomb ceramic carrier according to claim 1, wherein the addition amount of silicon carbide powder in the silicon inorganic powder is less than or equal to 83wt% and the balance is metal silicon powder, the addition amount of kaolin powder in the step 1 is less than or equal to 3% of the total weight of the silicon inorganic powder, and the pore-forming agent is less than or equal to 10% of the total weight of the silicon inorganic powder.
3. The method for preparing a thin-walled silicon carbide honeycomb ceramic carrier according to claim 2, wherein the silicon carbide powder has a particle size d50=24-30 μm and d100+.90 μm; the granularity D50=6-10 mu m and D100 is less than or equal to 25 mu m of the metal silicon powder; the kaolin powder is of a platy structure, the granularity D50=1-5 mu m and the D100 is less than or equal to 63 mu m; the pore-forming agent has a spherical structure, the granularity D50=20-40 μm and the granularity D100 is less than or equal to 75 μm.
4. The method for preparing a thin-walled silicon carbide honeycomb ceramic carrier according to claim 1, wherein the binder is added in an amount of 9-12% of the total weight of the silicon inorganic powder, and/or the binder is at least one of methylcellulose, hydroxypropyl methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyvinyl alcohol, clay, and bentonite.
5. The method for preparing a thin-walled silicon carbide honeycomb ceramic carrier according to claim 1, wherein the auxiliary agent is at least one of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent, and/or the addition amount of the auxiliary agent is 1-3% of the total weight of the silicon inorganic powder.
6. The method for preparing a thin-walled silicon carbide honeycomb ceramic carrier according to claim 1, wherein the lubricant in the step 2 is at least one of calcium stearate, white oil, base oil, glycerin, polyethylene glycol, synthetic fatty acid and water-soluble polyamide, and/or the amount of the lubricant added in the step 2 is 3-5% of the total weight of the silicon inorganic powder.
7. The method for preparing a thin-walled silicon carbide honeycomb ceramic carrier according to claim 1, wherein the conditions for the atmosphere sintering in step 4 are: under the protection of argon and reducing gas, the sintering temperature is raised to 1410-1450 ℃ from room temperature for heat preservation for 2-4h.
8. The method of claim 7, wherein the temperature rise rate during the atmosphere sintering from room temperature to 800 ℃ is less than 300 ℃/h, the temperature rise rate during the atmosphere sintering from 800 ℃ to 1100 ℃ is less than 10 ℃/h, and the temperature rise rate during the atmosphere sintering is less than 5 ℃/h.
9. A thin wall silicon carbide honeycomb ceramic carrier prepared by the method of any one of claims 1 to 8.
10. Use of a thin-walled silicon carbide honeycomb ceramic carrier according to claim 9 as a diesel particulate trap catalyst carrier.
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