Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
  • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
  • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
  • B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
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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
  • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
  • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
  • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
  • C04B35/478—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on aluminium titanates
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  • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
  • B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B28—WORKING CEMENT, CLAY, OR STONE
  • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
  • B28B1/00—Producing shaped prefabricated articles from the material
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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
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
  • C04B35/62625—Wet mixtures
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  • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
  • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
  • C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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  • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
  • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
  • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
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  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
  • C04B2235/3215—Barium oxides or oxide-forming salts thereof
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  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
  • C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • 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
  • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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  • C04B2235/36—Glass starting materials for making ceramics, e.g. silica glass
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  • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
  • C04B2235/54—Particle size related information
  • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
  • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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  • C04B2235/54—Particle size related information
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  • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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  • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
• • 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
  • F01N2330/00—Structure of catalyst support or particle filter
  • F01N2330/06—Ceramic, e.g. monoliths
• • 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
  • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
  • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
  • F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
  • F01N3/0222—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous the structure being monolithic, e.g. honeycombs

Definitions

• the invention generally relates to ceramic bodies.
• the invention relates to such ceramic bodies based on aluminum titanate.
• Such ceramic bodies are used, for example, as filter devices for
• Ceramic bodies can also be used as thermal insulation material.
• filters are made of a ceramic material, for example cordierite or silicon carbide. Find ceramic bodies made of cordierite
• cordierite In the filtration of diesel exhaust gases, cordierite has long been the material of choice as a low cost material that has a low thermal expansion coefficient. Porous cordierite ceramic filters have been used in the form of wall flow filters since the early 1980's to remove particulates in the exhaust flow of diesel engines.
• Wand Let usuate usually have a cylindrical shape with two end faces and a lateral surface and are traversed by the first end face to the second end face of a plurality of lying substantially parallel to the cylinder axis flow channels for the exhaust gases of diesel engines.
• the cross-sectional shape of the wall flow filter depends on the installation requirements of the motor vehicle. Widely used are filter bodies with a round, elliptical or triangular cross-section.
• the flow channels usually have a square or hexagonal cross section and are arranged in a narrow grid over the entire cross section of the filter body.
• a diesel particulate filter ideally combines a low thermal
• SiC silicon carbide
• aluminum titanate based ceramic filter elements have become known which have suitable properties for use at high temperatures (e.g., hot gas filtration), e.g. Vehicle exhaust control and diesel exhaust aftertreatment systems such as diesel particulate filter or particulate filter for
• Aluminum titanate is the stoichiometric mixed phase of alumina and titania. It is characterized by a low
• honeycomb structure with a plurality of honeycomb segments is known, which are connected to a unitary body.
• the major component of each of the honeycomb segments comprises at least one of silicon carbide, silicon nitride, cordierite, alumina, mullite, zirconia, zirconium phosphate, aluminum titanate, titanium dioxide, and combinations thereof.
• DE 10 2006 040 739 A1 discloses a filter for removing particles from a gas stream, in particular soot particles from an exhaust gas stream of an internal combustion engine, with a filter body made of a ceramic filter substrate, wherein the filter substrate with a porous protective layer of a coating material is coated.
• the coating material is selected from the group consisting of aluminum oxides, aluminum hydroxide, titanium dioxide, silicon dioxide, zirconium dioxide, cerium oxide, aluminum silicates, magnesium aluminum silicates, cordierite, mullite,
• Silicon carbide aluminum titanate, zeolites, quartz, glasses, mixtures and mixed oxides thereof.
• WO 2005/046840 discloses a ceramic body for use as a diesel particulate filter having a composition comprising:
• Blend a mineral phase such as barium, calcium and strontium feldspars.
• the ceramic body is molded by plastic molding techniques, e.g. Extruding, made.
• the disadvantage of this is that Feldsharite represent natural resources that
• Strontium feldspar is also extremely difficult to obtain. Further disadvantages of the barium, calcium and strontium feldspars are the high sintering temperature and the difficult ones
• such ceramic body or filter devices are also prepared in such a way that a non-combustible carrier web impregnated with a ceramic slurry and then a rigid filter body is formed.
• 63134020 A for example, describes a ceramic filter element for an exhaust gas filter in an internal combustion engine, which is constructed from a corrugated, spirally wound filter web.
• the filter web are heat-resistant,
• inorganic fibers mixed in an aqueous suspension with ceramic powder and to processed a web.
• Several superimposed webs are rolled up to the desired shape of the filter body, wherein honeycomb flow channels are formed between adjacent filter webs. The filter body is then fired at high temperature.
• WO 2006/005668 discloses another method for producing a ceramic filter element in an exhaust gas filter for internal combustion engines.
• a combustible, non-ceramic carrier web is first soaked with a ceramic slip and then burned out in the desired geometric shape until the
• Carrier track burned and a rigid filter body is formed.
• the invention is based on the object, ceramic body on the basis of
• Aluminum titanate to provide high thermal and chemical resistance, high long-term stability / decay resistance in reducing and oxidizing
• Atmosphere and good material properties have.
• the present invention achieves this object by providing a ceramic body based on aluminum titanate, which by adding special
• inorganic compounds is phase-stabilized, wherein the ceramic body has a specific composition. Furthermore, the object is achieved by providing a ceramic slurry which can be used for the production of the ceramic body.
• FIG. 1 shows a schematic representation of an internal combustion engine with a
• Filter device comprising a ceramic body according to the invention.
• Fig. 2 Viscosity curves of various formulations of the ceramic body according to the invention.
• Embodiment (s) of the invention The ceramic body according to the invention can be used, for example, as a catalyst. Above all, however, it can be used as a hot gas filter, liquid filter and especially as
• Diesel particulate filter or particulate filter can be used for a gasoline engine.
• the following is an example of the use as a diesel particulate filter described.
• FIG. 1 shows a schematic representation of an internal combustion engine with a filter device having a ceramic body according to the invention.
• the internal combustion engine 10 is connected via an exhaust pipe 12 in which the
• Filter device 14 is arranged with the ceramic body according to the invention. With the filter device 14 soot particles are filtered out of the exhaust gas flowing in the exhaust pipe 12. This is especially necessary in diesel engines to
• the filter device 14 comprises a cylindrical housing 16, in which, for example, a rotationally symmetrical, generally also cylindrical filter element 18 made of a ceramic body according to the invention is arranged.
• the filter element 18 comprises
• the ceramic body according to the invention has the following elemental composition (indicated as oxide):
• iii about 0.1 to about 5.0 wt% MgO; iv) 0 - about 2.0 wt.% Fe 2 O 3 ; v) 0 - about 1.0 wt.% BeO, BaO or CaO; vi) 0 - about 1.0 wt .-% Li 2 0, Na 2 0 or
• the ceramic body according to the invention has the following elemental composition (indicated as oxide):
• the ceramic body according to the invention has the following elemental composition (indicated as oxide):
• oxide elemental composition
• the ceramic body according to the invention has the following composition: 1.> 95 wt .-% (A1 2 0 3 ⁇ Ti0 2 ); 2. 0, 1 - 5 wt .-% Si0 2 ; 3. 0.7-5 wt.% MgO; 4. 0-2% by weight Fe 2 O 3 ; 5. 0-1% by weight of CaO; and 0.1-2% by weight impurities.
• the ceramic body according to the invention has the following composition: 1.> 95 wt .-% (A1 2 0 3 ⁇ Ti0 2 ); 2. 0, 1 - 5 wt .-% Si0 2 ; 3. 0.7-5 wt.% MgO; 4. 0-2% by weight Fe 2 O 3 ; 5. 0-1% by weight of CaO; and 0.5-2% by weight impurities.
• MgO serves to stabilize the aluminum titanate phase under reducing conditions in the critical temperature range of about 900 ° C-1300 ° C.
• MgO source come, for example, MgTi0 3 , Mg 2 Ti0 4 , MgTi 2 0 5 and MgAl 2 0 4 in question.
• Si0 2 or optionally additionally also CaO or Fe 2 0 3 is advantageous for the stabilization of the aluminum titanate phase under oxidizing conditions in critical temperature range of about 900 ° C-1300 ° C.
• the stabilization of the phase is determined by measuring and comparing the thermal expansion coefficient (CTE) before and after the aging. All WAK measurements listed here were carried out by means of an ETZSCH push rod dilatometer - Model 402 C with a heating rate of 5 K / min under air atmosphere in a Netzsch application laboratory.
• Si0 2 is also important for increasing the mechanical strength of the ceramic bodies on aluminum titanate B asi s.
• Si0 2 source is the use of a CaO glass frit.
• glass frits of the types 40 580 TF, 10 083 or 10 1911-D from Ferro are used.
• SiO 2 which is in a range from about 0.1 to about 5.0% by weight is advantageous.
• Particularly preferred ranges of Si0 2 are between about 1.0 to about 4.5 weight percent, between about 1.0 and about 4.0 weight percent, and between about 2.5 and about 3.6 weight percent. -%, and between about 3.0 and about 3.1 wt .-%.
• iron oxide is present in the ceramic body, it is preferably used in amounts ranging from about 0.1 to about 1.1 wt%. Be particularly advantageous amounts of Fe 2 0 3 have proven between about 0.2 and about 0.3 wt .-%.
• the ratio of A1 2 0 3 to Ti0 2 in the aluminum titanate is designed so that a mass ratio of Ti0 2 : Al 2 0 3 is in the range of about 0.75 to about 0.95.
• a ratio has been found in which a molar excess of titanium dioxide is present such as a mass ratio Ti0 2 : Al 2 0 3 of> 0.8 (molar ratio> 1.02).
• mass ratios of TiO 2 : Al 2 O 3 between about 0.80 and about 0.90, and between about 0.80 and about 0.85, and between about 0.81 and about 0.82 proved.
• a ceramic body according to the invention can be produced by plastic forming methods, such as e.g. Extruders are produced.
• plastic forming methods such as e.g. Extruders are produced.
• a ceramic slip it is also possible to impregnate a non-ceramic carrier web with a ceramic slip and then burn out in the desired geometric shape until the carrier web is burned and a rigid filter body is formed.
• Slurry properties such as a better rheology, which is characterized by eg a viscosity of less than about 0.2 Pa s.
• the viscosity is less than about 0.1 Pa s, less than about 0.05 Pa s, and less than about 0.02 Pa s.
• the viscosity was measured with a Brookfield rheometer type RVDV III + CP with cone / plate (cone 42) between 5 and 100 revolutions per minute at a temperature of about 25 ° C.
• the viscosity was measured between 5 to 30 revolutions per minute or between 15 to 25 revolutions per minute, eg at 20 revolutions per minute.
• the properties that characterize better rheology also include increased long-term stability, as well as a higher solids content (FSG), etc. Without being bound to a particular theory, it is believed that the reason for the improved properties is the avoidance of the formation of Mg 2+ ions in the ceramic slurry. These 2-fold charged Mg ions lead to a strong increase in the charge density in the electrical
• Double layer thickness reduced so far that the attractive interactions (van der- Waals attraction) dominate over the repulsive forces, occurs coagulation of the particles and possibly also on particle sedimentation.
• curve Sl and S6 are basically for the production of filter bodies on the o.g. Impregnation technique suitable. However, it may occur that the channels of the filter body run and thus block the pore structure, which is not preferred. Under the increased long-term stability of the slurry is understood in particular a substantially unchanged viscosity over a period of 12 h, 24 h, preferably 48 h. Under one in
• Substantially unchanged viscosity is understood to mean that said change in viscosity is in a range of less than about ⁇ 20%, preferably in a range of less than about ⁇ 10%, even more preferably in a range of less than about ⁇ 5%. In a preferred embodiment, no substantial or no sedimentation occurs for a period of more than 12 hours, 24 hours, preferably more than 48 hours. The increased long-term stability enables production with consistent quality and high efficiency.
• an amount of MgO which is in a range from about 0.4 to about 3.0% by weight has proven advantageous for the ceramic body.
• amounts of MgO have been found to be between about 0.5 and about 1.5 weight percent, and between about 0.8 and about 1.3 weight percent, between about 0.9 and about 1.3 Wt .-%, between about 0.9 and about 1.1 wt .-%.
• the ceramic body of the present invention may have a porosity between about 25% and about 70%.
• the porosity is between about 30% and about 60%, more preferably between about 35% and about 55%.
• the porosity of the ceramic body is determined by means of mercury (Hg) porosimetry, device type, for example, the device Pascal 140/440 Thermo Fischer was used.
• the median pore radius may be between about 0.1 ⁇ and about 20.0 ⁇ , more preferably between about 1.0 ⁇ and about 20.0 ⁇ , more preferably between about 10.0 ⁇ and about 18.0 ⁇ further preferred between about 13.0 ⁇ and about 17.0 ⁇ and most preferably between about 14.5 ⁇ and about 15.5 ⁇ amount.
• the mean pore radius and the median pore radius is determined by means of Hg porosimetry, the device type Pascal 140/440 from Thermo Fischer was used. Alternatively, for measuring the
• the present invention also relates to a ceramic slurry.
• the slip according to the invention has the following in one embodiment
• the alcohol is selected from the group consisting of methanol, ethanol, isopropanol, butanol, glycerol, ethylene glycol, n-propyl alcohol, n-hexyl alcohol, secondary butyl alcohol, isobutyl alcohol, tertiary butyl alcohol, trimethylcarbinol, isoamyl alcohol, 1,2-glycol, propylene glycol, Trimethylene glycol, tetramethylene glycol, hexamethylene glycol, octamethylene glycol, nonamethylene glycol or the like.
• the stated percentages by weight are based on the dry mass of the slip, without addition of the solvent.
• Ceramic slips refer to the proportions of the respective
• Metal oxides If a component in the ceramic slurry is not present in the form of the oxide, then the proportion of the respective metal or metal ion to the amount of its Oxide related. If, for example in the slurry an Mg 2+ ion and / or MgTi0 3, Mg 2 Ti0 4, MgTi 2 0 5, MgAl 2 0 4 is present, the wt .-% given are for MgO.
• Dispersing aid ranging from about 0.1 to about 4.0% by weight. Amounts of dispersing aid have proven to be particularly advantageous between about 0.1 and about 3.0% by weight. Suitable dispersants are for example C 20 acids or carboxylic acids, Carbonklareester, and salts of polycarboxylic or polyacrylic acid preparations or mixtures of the foregoing. A preferred dispersing aid is Dolapix CE64 from Zschimmer & Schwarz,
• Ceramic slip comprising an amount of A1 2 0 3 between about 52.0 and about 55.0 wt .-%, preferably between about 53.0 and about 54.0 wt .-% A1 2 0 3 .
• a ceramic slurry comprising an amount of TiO 2 between about 42.0 and about 43.0 wt% TiO 2 , preferably between about 42.0 and about 42.2 wt% TiO 2 .
• Ceramic slurry comprising an amount of Si0 2 between about 2.0 and about 3.0 wt .-% Si0 2 , preferably between about 2.7 and about 2.9 wt .-% Si0 2 .
• a ceramic slurry comprising an amount of MgO between about 1.0 and about 2.0 wt.% MgO, preferably between about 1.2 and about 1.5 wt.% MgO.
• the solids content of the slip of the present invention should preferably range from about 45 to about 75%. Most preferably, a solids content has been found to be between about 55 and about 75 percent, most preferably between about 58 and about 68 percent.
• Improved rheology of the slurry can have a positive effect on the properties of the ceramic slurry.
• a ceramic slip is preferred Slip having a viscosity of less than about 0.2 Pa s, preferably less than about 0.1 Pa s, more preferably less than about 0.05 Pa s and most preferably less than about 0.02 Pa s.
• the viscosity of the slurry is measured with a Brookfield rheometer type RVDV III + CP with cone / plate (cone 42) between about 5 and 100 revolutions per minute at a temperature of about 25 ° C.
• the constituents of the ceramic slurry preferably have suitable particle size distributions, so that they can penetrate into the pores of the carrier material.
• the AI 2 O 3 component of the ceramic slurry preferably has a particle size distribution d 90 between approximately 0.1 ⁇ m and approximately 4.0 ⁇ m. Particularly advantageous is a particle size distribution d90 has been found between about 1.0 and about 3.0 ⁇ , more preferably between about 2.0 and about 3.0 ⁇ and most preferably between about 2.5 and about 2.8 ⁇ .
• a particle size distribution d90 has been found between about 1.0 and about 3.0 ⁇ , more preferably between about 2.0 and about 3.0 ⁇ and most preferably between about 2.5 and about 2.8 ⁇ .
• the A1 2 0 3 component of the ceramic slurry has a particle size distribution d50 between about 0.1 ⁇ and about 1.5 ⁇ .
• a particle size distribution d50 has been found between about 0.1 and about 1.0 ⁇ , more preferably between about 0.4 and about 0.8 ⁇ and most preferably between about 0.6 and about 0.8 ⁇ .
• Particle size distribution d90 and d50 refers to the volume distribution.
• the TiO 2 component of the ceramic slurry preferably has a particle size distribution d90 between approximately 0.1 ⁇ m and approximately 1.0 ⁇ m. Particularly advantageous is a particle size distribution d90 between about 0.2 and about 0.8 ⁇ proven, preferably between about 0.4 and about 0.6 ⁇ and most preferably between about 0.5 and about 0.6 ⁇ .
• the Ti0 2 component of the ceramic slurry has a particle size distribution d50 between about 0.1 ⁇ and about 1.0 ⁇ . Particularly advantageous is a particle size distribution d50 has been found between about 0, 1 and about 0.5 ⁇ and most preferably between about 0.2 and about 0.3 ⁇ .
• the glass frit as Si0 2 source which is added to the ceramic slurry, preferably has a particle size distribution d90 between about 5.0 ⁇ and about 20.0 ⁇ on. Particularly advantageous is a particle size distribution d90 between about 10.0 and about 15.0 ⁇ proven, preferably between about 13.0 and about 14.0 ⁇ and most preferably between about 13.0 and about 13.5 ⁇ .
• the glass frit as Si0 2 component of the ceramic slurry has a particle size distribution d50 between about 0, 1 ⁇ and about 10.0 ⁇ on.
• a particle size distribution d50 between about 2.0 and about 8.0 ⁇ proven, preferably between about 6.0 and about 7.0 ⁇ and most preferably between about 6.4 and about 6.6 ⁇ .
• the MgO source (eg added as MgTi0 3 , Mg 2 Ti0 4 , MgTi 2 0 5 or MgAl 2 0 4) of the ceramic slurry preferably has a particle size distribution d90 between about 0.1 ⁇ and about 5.0 ⁇ .
• a particularly advantageous has a
• the MgO source of the ceramic slurry preferably has a particle size distribution d50 between approximately 0.1 ⁇ m and approximately 5.0 ⁇ m.
• Particularly advantageous has a particle size distribution d50 between about 1.0 and about 3.0 ⁇ proven, preferably between about 1.0 and about 2.0 ⁇ and most preferably between about 1.2 and about 1.4 ⁇ .
• a ceramic slip has proved to be advantageous, which is characterized in that the particles are present in the mixture as non-agglomerated particles with d90 values of less than approximately 3.2 ⁇ m. Not particularly advantageous
• Non-agglomerated particles with d90 values less than about 2.0 ⁇ proven, preferably less than about 1.0 ⁇ and most preferably less than about 0.3 ⁇ .
• the particles in the mixture as non-agglomerated particles have a d50 value of less than approximately 0.4 ⁇ m.
• Non-agglomerated particles having d 50 values of less than about 0.3 ⁇ m, preferably less than about 0.2 ⁇ m, and most preferably less than about 0.1 ⁇ m, have proven to be particularly advantageous.
• Non-agglomerated particles are particles which have been ground up to size on primary particles and are also present as such disperse in the slurry.
• the ceramic slurry may contain proportionally nanoscale particles less than 100 nm in size.
• the starting ceramic slurry contains organic additives, e.g. organic polymers, e.g. Polyvinyl acetate (PVA),
• organic polymers e.g. Polyvinyl acetate (PVA)
• Polyvinylpyrrolidone PVP
• polyamides polystyrenes, polyurethanes, polypropylene,
• Schlicker suitable thixotropic agents, wetting agents, pore formers, defoamers and rheology additives or combinations thereof are added. These additives can be added in each case in an amount of 0-5 wt .-%, preferably from 0 to 2.5 wt .-%, wherein the weights are based on the total weight of the slurry, without the solvent content.
• additives can be added either singly or in combination.
• the addition of these substances has a positive influence on the slip rheology as well as the flow and wetting properties result and allows a targeted adjustment of the porosity and pore size / distribution, which leads to an improvement in filter performance, component homogeneity and mechanical strength.
• these additives improve the infiltration behavior of the slips in the paper and the adhesion of the individual ceramic particles to the paper fibers and thus enable a targeted improvement of wet-ceramized paper body to avoid drying damage, such as cracks, Schlickerauswaschungen, structural inhomogeneities, etc.
• a shaping of the body is possible either before or after soaking with the ceramic slurry.
• thixotropic agents all substances which cause a thixotropic behavior of liquids are referred to as thixotropic agents.
• suitable thixotropic agents are solutions of modified ureas, such as a solution of (BYK-420 from BYK Chemie.
• the pore-forming agent is any substance which is added to the slurry and which leads to the formation of pores in the finished ceramic body.
• suitable pore formers are carbon or polymers such as e.g. Polyamides, polystyrenes, polyurethanes, polypropylene, polyethylene, polyvinyl acetate, polyvinylpyrrolidone, acrylates, and starch or other wheat starch and wood flour, or combinations of the foregoing.
• polyamide is used with a size of 0.5 - 90 ⁇ such. Vestosint 2070 natural color (Evonik).
• wetting agent refers to any substance which is added to the slurry in order to improve the wetting and wettability of the material
• wetting agents are used to increase the contact between carrier webs (solid phase) and slip (liquid phase), as well as the
• suitable wetting agents are modified siloxanes, such as e.g. polyether-modified siloxane such as e.g. BYK-348 from BYK Chemie or non-ionic solutions of an acrylate copolymer such as e.g. BYK-380N from BYK Chemie.
• modified siloxanes such as e.g. polyether-modified siloxane such as e.g. BYK-348 from BYK Chemie or non-ionic solutions of an acrylate copolymer such as e.g. BYK-380N from BYK Chemie.
• any substance is added which is added to the slurry in order to increase the rheology properties of the slurry.
• Defoamer for the purposes of the present invention is any substance which is added to the slurry in order to avoid foaming.
• An example of a suitable defoamer is a mixture of polysiloxanes and hydrophobic solids in polyglycol, such as: BYK-028 from BYK Chemie, which is a mixture of a polysiloxane and hydrophobic solids in polyglycol.
• the amount of antifoaming agent is preferably between about 0 and about 0.5% by weight, based on the total slip including the solvent.
• Another criterion for evaluating the properties of the ceramic slurry is electrical conductivity, which indicates the ability of the ceramic body
• an electrical conductivity of the ceramic slurry of the present invention which is less than 1500 ⁇ 8 / ⁇ , preferably less than 1000 ⁇ 8 / ⁇ , more preferably less than 800 ⁇ 8 / ⁇ , and most preferably less than 600 ⁇ / ⁇ .
• the present invention is also directed to a method of making a
• directed ceramic body comprising the following steps: (a) providing a combustible, non-ceramic carrier web, (b) impregnating the carrier web with a ceramic slurry, (c) optionally pyrolysis of the carrier web, (d) sintering under oxidic and / or non-oxidic atmosphere and thus formation of a rigid body.
• the carrier web is any web which is suitable for being wetted by a slurry.
• the carrier web can off
• the carrier web may be selected from synthetic material, wherein the synthetic material preferably comprises plastic fibers.
• the carrier web is brought into the desired geometric shape, which is preferably maintained during the process.
• the method of manufacturing a ceramic body involves the use of a ceramic slurry of the present invention.
• the ceramic slip can be ground until a desired particle size is achieved.
• the constituents of the ceramic slurry can be ground until a particle size distribution d90 of less than about 3.2 ⁇ is reached, preferably less about 2.0 ⁇ , more preferably less about 1.0 ⁇ and most preferably less about 0, 3 ⁇ .
• the constituents of the ceramic slurry can be ground until a
• Particle size distribution d50 of less than about 0.4 ⁇ is achieved, preferably less about 0.3 ⁇ , more preferably less about 0.2 ⁇ and most preferably less than about 0.1 ⁇ .
• a stirred ball mill can be used to grind the ceramic slurry.
• the step (b) of the method for producing a ceramic body according to the present invention comprises soaking the carrier web with a ceramic slurry for less than about 10 minutes, more preferably less than about 5 minutes, more preferably less than about 2 minutes more preferably less than about 1.5 minutes, and most preferably less than about 1 minute.
• the impregnated carrier web can be drained off after process step (b).
• the impregnated carrier web can be turned during draining, preferably being turned twice.
• the dripping time is approximately less than 1 hour, preferably less than about 45 minutes, and most preferably less than about 30 minutes.
• the impregnated carrier web can be additionally dried after dripping after process step (b).
• the drying of the impregnated carrier web comprises about 20 minutes to about 6 hours, preferably about 40 minutes to about 4 hours, most preferably about 1 to about 3 hours.
• the drying of the impregnated carrier web may comprise electromagnetic radiation, preferably
• the drying of the impregnated carrier web can be carried out in a continuous dryer and / or in a drying oven.
• the optional step (c) of the method for producing a ceramic body according to the present invention comprises the pyrolysis of the dried ones
• Carrier web wherein the pyrolysis is preferably carried out under an inert gas atmosphere.
• the inert gas atmosphere comprises nitrogen, argon and / or all noble gases, as well as combinations thereof).
• the pyrolysis takes place at a temperature between about 20 and about 1000 ° C, preferably at about 1000 ° C. In a further preferred embodiment, the pyrolysis is carried out for a period between about 1 and about 10 hours, preferably between about 2 and about 6 hours.
• the skilled person can the required pyrolysis time depending on Adjusting the maximum temperature, ie comparable or identical results at lower temperatures such as 800 ° C, if the period is adjusted accordingly.
• the step (d) of the method for producing a ceramic body according to the present invention includes burnout, with sintering being preferred.
• the sintering can take place in an oxidizing atmosphere.
• the burnout of the carrier web comprises a maximum temperature between about 1000 ° C and 2000 ° C, more preferably between about 1200 ° C and 1800 ° C, more preferably between about 1300 ° C and 1600 ° C, and most preferably between about 1360 ° C and 1500 ° C.
• an outer layer may be applied to the rigid filter body.
• the materials used for the outer layer include the same material as the filter body or a
• Aluminosilicate cements such as e.g. the ceramic cement CC 180W from Ceprotec or a mixture of special filter material (aluminum titanate) and an aluminum silicate ceramic cement as binder.
• aluminum titanate aluminum titanate
• aluminum silicate ceramic cement as binder.
• the outer layer used material comprises one of the embodiments disclosed in the documents DE102009001820A1, DE102009010207A1, EP000001688171B1, US000007560154B2, US000007591918B2, US000007651755B2, US020090286041A1, and WO002009070250A1.
• the method further comprises the step of sawing off the end faces of the ceramic body.
• the ceramic body according to the invention consists of a temperature-resistant material and is therefore z. B. suitable for use as a diesel particulate filter.
• the material properties can be better influenced and the microstructural properties adjusted better.
• the filter device according to the invention shows a good thermal shock resistance and a low thermal expansion.
• the coefficient of thermal expansion is a parameter that describes the behavior of a substance with respect to changes in its dimensions when the temperature changes.
• CTE coefficients of thermal expansion
• Aluminum titanate has CTE values of 1.0 * 10-6 1 / K (20-1000 ° C) without thermal aging and even 4.2 * 10-6 1 / K (20-1000 ° C) after thermal aging into oxidizing Atmosphere (same conditions as in the above table) measured.
• the thermal expansion coefficients for the ceramic bodies of the present invention before swapping are between about -0.5 and about 2.0 * 10 -6 " 1 / K, preferably between about -0.5 and about 1.5 * 10 -6 " / K, more preferably between about -0.5 and about 1.2 x 10 -6 1 / K, and most preferably between about -0.5 and about 0.6 * 10 -6 1 / K, in a range from about 20 ° C - 1000 ° C.
• the coefficient of thermal expansion of the present invention be in a range of about 20 ° C - 1000 ° C values is between about -0.5 * 10 "6 to about 2.0 x 10" 6 1 / K, preferably, between about -0.5 and about 1.5 * 10 "6 1 / K, more preferably between about -0.5 and about 1.2 * 10" 6 1 / K, and most preferably between about -0.5 and about 0 , 8 * 10 "6 1 / K or in a range of 20 ° C - 800 ° C values is between about -0.5 * 10" 6 to about 2.0 x 10 "6 1 / K, preferably between about -0 , 5 and about 1.2 * 10 "6 1 / K, more preferably between about -0.5 and about 1.0 * 10 -6 1 / K, and most preferably between about -0.5 and about 0.6 * 10 "6 1 / K.
• the aging under oxidizing conditions can be carried out, for example, in air for a period of 40 hours
• the coefficient of thermal expansion of the present invention be in a range of about 20 ° C - 1000 ° C values is between about -0.5 * 10 "6 and about 2.4 x 10" 6 1 / K, preferably, between about -0.5 and about 2.0 * 10 "6 1 / K, more preferably between about -0.5 and about 1.7 * 10" 6 1 / K, and most preferably between about 0.5 and about 1.5 * 10 "6 1 / K or in a range of 20 ° C - 800 ° C values between about -0.5 * 10 " 6 and about 2.4 x 10 -6 1 / K, preferably between about -0.5 and about 1.7 * 10 -6 " 1 / K, more preferably between about -0.5 and about 1.5 * 10 -6 1 / K, and most preferably between about -0.5 and about 1.0 * 10 -6 1 / K.
• the aging under reducing conditions can be carried out, for example, in a CO atmosphere for a period of 20 hours at 1050 ° C (
• the viscosity curve of the formulation S1 shows a pseudoplastic behavior, ie a decreasing viscosity with an increase in the shear rate.
• the cause is the use of illite as the Si0 2 and iron source.
• This clay mineral contains besides Si0 2 , A1 2 0 3 and Fe 2 0 3 also foreign substances such as MgO, CaO, etc.
• foreign substances such as Mg 2+ , Ca 2+ , etc.
• pseudoplastic behavior of the slip system Sl is based on compression of the electric double layer by the presence of polyvalent counterions (Mg 2+ ). These originate from the used MgO source (MgO or MgTi0 3 ). This behavior is very unfavorable for the impregnation process of paper wraps, since during the impregnation process and during subsequent drying hardly or no shear forces act on the slurry. As a result, the slip viscosity remains high and the slip surplus runs badly from the winding after the impregnation process. Thus, ceramic layers with low porosity form in the channels, which greatly increases the pressure loss of the component. Consequently, inventive ceramic bodies produced from the formulation S1 exhibit considerable inhomogeneities (inhomogeneous structure or porosity, etc.), as well as frequently macroscopic defects (accrued channels, cracks, deformations, etc.). The pronounced
• Intrinsic viscosity of the slip formulation S6 results from a crosslinking reaction of the silica sol used (Si0 2 source). This aging process is noticeable after a very short time ("lh). The polysilicic acid particles form Si-O-Si bonds among each other, resulting in gelation of the entire ceramic slurry.
• the viscosity curves of the formulations S14 and S15 show only a very slight or no shear-thinning behavior (Newtonian viscosity behavior).
• the slip process after the impregnation process is greatly facilitated so that no or hardly any ceramic layers block the porous bulk structure of the channels.
• Magnesium titanate was used as the source of MgO in formulas S14 and S15, which prevents Mg 2+ ions from dissolving.
• the mechanical properties of components based on the Formulations S14 and S15 for example, fully meet the requirements for diesel particulate filters and particulate filters for gasoline engines. The bursting pressures of corresponding filters can reach> 10 bar.
• Wetting agent or combinations thereof.
• the following properties can be positively influenced both by the ceramic slip systems and by the ceramic bodies produced therefrom: rheological properties, homogeneity,
• Step 1 Production of the basic loader
• Dolapix CE64 Zschimmer & Schwarz
• 36.4 kg of demineralized water as a dispersant.
• 43.332 kg A1 2 0 3 type APA-05, Sasol
• 34.056 kg Ti0 2 type X200, Kemira
• 2.48 kg MgTi0 3 magnesium titanium oxide, 99% metal base, Alfa Aesar, Johnson Mattey
• 3.593 kg of a glass frit type 10191 1, Ferro
• the slurry After stirring for 5 hours, the slurry is ground by means of a stirred ball mill, the total energy input being approximately 13.0 kWh. After grinding, the electrical conductivity of the slurry is about 500 to about 550 ⁇ 8 / ⁇ , where the pH is about 8.6. Then the slurry is stirred for about 2 hours.
• Step 2 Making the diver
• the Luvitec K-90 solution can be prepared by dissolving 20% by weight of Luvitec K 90 powder (BASF) in 80% by weight of water.
• the mixture is stirred vigorously for about 2 hours and then slowly stirred for about 1 hour.
• Step 3 soaking process
• a paper blank (reel) is selected which is submerged for about 30 seconds in the ready-to-stir dipping schicker obtained from step 2. Subsequently, the soaked paper roll is drained for about 30 minutes under room conditions, turning the paper roll after about 15 minutes each.
• the soaked carrier web is dried for about 20 to about 30 minutes in a microwave or radio wave dryer at about 100-130 W microwave power (per component).
• the dried carrier web is dried for a period of about 48 to about 72 hours in a climatic chamber at about 60 ° C and about 10% relative humidity.
• Step 5 Pyrolysis Subsequently, the dried carrier web is pyrolyzed under an inert gas atmosphere at 1000 ° C. with a holding time of 6 hours.
• Step 6 Sintering process
• a sintering process is performed under an oxidizing air atmosphere at a temperature between about 1400 ° C and about 1600 ° C for a period of about 5 to 20 hours.

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