WO2024097048A1 - Procédé d'induction d'un état de traînée de paroi réduite dans une pâte de précurseur céramique à traînée de paroi élevée - Google Patents

Procédé d'induction d'un état de traînée de paroi réduite dans une pâte de précurseur céramique à traînée de paroi élevée Download PDF

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WO2024097048A1
WO2024097048A1 PCT/US2023/035753 US2023035753W WO2024097048A1 WO 2024097048 A1 WO2024097048 A1 WO 2024097048A1 US 2023035753 W US2023035753 W US 2023035753W WO 2024097048 A1 WO2024097048 A1 WO 2024097048A1
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amount
component
mixture
inorganic
weight
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Keith Norman BUBB
Michael James LEHMAN
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Corning Incorporated
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    • C04B35/16—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 silicates other than clay
    • C04B35/18—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 silicates other than clay rich in aluminium oxide
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    • 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
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    • 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
    • C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B35/634—Polymers
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
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    • 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
    • C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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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
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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
    • C04B2235/3231—Refractory metal 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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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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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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Definitions

  • the present specification relates to ceramic pastes (ceramic and/or ceramicforming pastes), methods of making such pastes, and methods of making self-standing extruded articles by extruding such pastes.
  • Ceramic products in a wide range of fields from refractory tubing to automotive and diesel exhaust filters and catalytic converter substrates can be manufactured by extrusion of pastes. The cost of such products can be driven by the rate of production of quality products.
  • a method of manufacturing a ceramic-forming batch mixture comprising: changing a cordierite precursor batch mixture (“starting mixture”) from a high wall drag state (“first state”) to a reduced wall drag state (“second state”) by introducing an amount of one or more lubricant constituents in the batch mixture (“resulting batch mixture”).
  • the resulting batch mixture in the second state exhibits a lower wall drag than the starting mixture in the first state, as measured via the same capillary rheometer test.
  • the second state is not a low drag wall state.
  • the introducing the amount of one or more lubricant constituents comprises adding, or increasing, an amount of PEO.
  • the starting mixture comprises: an inorganic component comprised of cordierite precursor inorganic particles; a cellulosic binder component comprised of a methylcellulose constituent; a lubricant component comprised of fatty acid and/or synthetic oil; and a liquid vehicle component comprised of water.
  • the resulting mixture comprises a higher amount of PEO, and a lower amount of the methylcellulose constituent.
  • the starting mixture contains no PEO.
  • the starting mixture contains fatty acid and synthetic oil.
  • the starting mixture contains greater than 0.5 wt% fatty acid and greater than 5.00 wt% synthetic oil.
  • the starting mixture contains less than 2.00 %fatty acid and less than 7.00 wt% synthetic oil.
  • the resulting mixture contains no synthetic oil.
  • the resulting mixture contains 1.00 to 3.00 wt% PEO.
  • the cellulosic binder component comprises methylcellulose. In some embodiments, the cellulosic binder component consists of methylcellulose.
  • the PEO has a molecular weight of 1 million or more. In embodiments, the PEO has a molecular weight of 1-2 million.
  • the PEO has a molecular weight of 2 million or more. In embodiments, the PEO has a molecular weight of 5 million or more. In embodiments, the PEO has a molecular weight of 7 million or more.
  • the synthetic oil comprises a polyalphaolefin.
  • the PEO has a molecular weight of 5 million or less. In embodiments, the PEO has a molecular weight of 2 million or less. In embodiments, the PEO has a molecular weight of 1 million or less.
  • a ceramic batch mixture comprising: an inorganic component in an inorganic amount; a binder component in a binder amount measured as a super addition by weight to the inorganic amount, the binder component comprising a cellulose-based polymer component in a cellulosic amount measured as a super addition by weight to the inorganic amount; and a polyethylene oxide component in a polyethylene oxide amount measured as a super addition by weight to the inorganic amount; a pore former component in a pore former amount measured as a super addition by weight to the inorganic amount; and a liquid component in a liquid amount measured as a super addition by weight to the inorganic amount, the liquid component comprising water; wherein the ceramic batch mixture exhibits wall drag which differs by less than 15% between temperatures of 20 to 40 C, inclusive, at extrusion velocities between 0.5 and 2.5 inch/second, inclusive, as measured by capillary rheometer.
  • a method of preparing a ceramic batch mixture comprising: mixing together an inorganic component in a first inorganic amount, a binder component in a first binder amount measured as a super addition by weight to the first inorganic amount, the binder component comprising a cellulose-based polymer component in a first cellulosic amount measured as a super addition by weight to the first inorganic amount, a pore former component in a first pore former amount measured as a super addition by weight to the first inorganic amount, and a liquid component in a first liquid amount measured as a super addition by weight to the first inorganic amount, the liquid component comprising water, wherein the mixing produces a first batch mixture.
  • the method may further comprise preparing the ceramic batch mixture by mixing together: the inorganic component in the first inorganic amount, the pore former component in the first pore former amount measured as a super addition by weight to the first inorganic amount, a binder component in a second binder amount measured as a super addition by weight to the first inorganic amount, the binder component comprising a cellulose-based polymer component in a second cellulosic amount measured as a super addition by weight to the first inorganic amount, the binder component further comprising a polyethylene oxide component in a polyethylene oxide amount measured as a super addition by weight to the first inorganic amount, wherein the second cellulosic amount is less than the first cellulosic amount, and the liquid component in a second liquid amount measured as a super addition by weight to the first inorganic amount, in such amounts that the ceramic batch mixture is in a reduced wall drag state wherein the ceramic batch mixture exhibits a wall drag greater than 5 and less than 16 psi at velocities between
  • the method may further comprise preparing one or more subsequent ceramic batch mixtures by replacing a portion of the cellulose-based polymer component with the polyethylene oxide component in a polyethylene oxide amount measured as a super addition by weight to the inorganic amount, thereby adjusting wall drag of the ceramic batch mixture.
  • the ceramic batch mixture exhibits a wall drag greater than 7 and less than 16 psi at velocities between 0.5 and 2.5 inch/second as measured by capillary rheometer.
  • the ceramic batch mixture exhibits a wall drag greater than 10 and less than 25 psi at velocities between 1.0 and 2.5 inch/second as measured by capillary rheometer.
  • a sample of the ceramic batch mixture exhibits a strain at break (SAB) of greater than 13 %. In embodiments, a sample of the ceramic batch mixture exhibits a strain at break (SAB) of greater than 15 %. In embodiments, a sample of the ceramic batch mixture exhibits a strain at break (SAB) of 13 to 20%.
  • the ceramic batch mixture exhibits wall drag which differs by less than 15% between temperatures of 20 to 40 C, inclusive, at extrusion velocities between 0.5 and 2.5 inch/second, inclusive, in a capillary rheometer.
  • the cellulose-based polymer comprises a cellulose ether.
  • the cellulose ether comprises one or more of methylcellulose (MC), hydroxypropylcellulose or hydroxypropylmethylcellulose (HPMC) and hydroxyethylmethylcellulose (HEMC).
  • the cellulose-based polymer comprises methylcellulose.
  • the ceramic batch mixture further comprises a lubricant component in a lubricant amount less than 1% by weight superaddition to the inorganic amount.
  • the lubricant component comprises a synthetic lubricant in an amount less than 1% by weight superaddition to the inorganic amount.
  • the lubricant component is free of synthetic lubricant.
  • the lubricant component comprises an oil lubricant.
  • the oil lubricant comprises one or more of light mineral oil, corn oil, high molecular weight polybutenes, polyol esters, a blend of light mineral oil and wax emulsion, a blend of paraffin wax in corn oil, and combinations of these.
  • the amount of oil lubricants is from about 1% by weight to about 10% by weight. In an exemplary embodiment, the oil lubricants are present from about 3% by weight to about 6% by weight.
  • the pore former component comprises one or more of a starch, graphite, polymer resin, or combinations thereof.
  • the ceramic batch mixture further comprises a surfactant component in a surfactant amount less than 1% by weight superaddition to the inorganic amount.
  • the surfactant component comprises one or more of C8 to C22 fatty acids, and/or their derivatives, C8 to C22 fatty esters, C8 to C22 fatty alcohols, and combinations of these.
  • the surfactant component comprises stearic, lauric, myristic, oleic, linoleic, palmitic acids, and/or their derivatives, tall oil, stearic acid in combination with ammonium lauryl sulfate, and combinations of all of these.
  • the surfactant component comprises lauric acid, stearic acid, oleic acid, tall oil, and combinations of these. In some embodiments, the amount of surfactants is from about 0.25% by weight to about 2% by weight as a super addition to the inorganic component.
  • a ceramic batch mixture comprising: an inorganic component in an inorganic amount; a binder component in a binder amount measured as a super addition by weight to the inorganic amount, the binder component comprising a cellulose-based polymer component in a cellulosic amount measured as a super addition by weight to the inorganic amount; and a polyethylene oxide component in a polyethylene oxide amount measured as a super addition by weight to the inorganic amount; a pore former component in a pore former amount measured as a super addition by weight to the inorganic amount; and a liquid component in a liquid amount measured as a super addition by weight to the inorganic amount, the liquid component comprising water; wherein the ceramic batch mixture exhibits a wall drag greater than 5 and less than 16 psi at velocities between 0.5 and 2.5 inch/second as measured by capillary rheometer.
  • the ceramic batch mixture exhibits a wall drag greater than 7 and less than 16 psi at velocities between 0.5 and 2.5 inch/second as measured by capillary rheometer. [0028] In embodiments, the ceramic batch mixture exhibits a wall drag greater than 10 and less than 25 psi at velocities between 1.0 and 2.5 inch/second as measured by capillary rheometer.
  • a sample of the ceramic batch mixture exhibits a strain at break of greater than 13 %.
  • a sample of the ceramic batch mixture exhibits a strain at break of greater than 15 %.
  • a sample the ceramic batch mixture exhibits a strain at break of 13 to 20%.
  • the ceramic batch mixture exhibits wall drag which differs by less than 15% between temperatures of 20 to 40 C, inclusive, at extrusion velocities between 0.5 and 2.5 inch/second, inclusive, in a capillary rheometer test.
  • the cellulose-based polymer comprises a cellulose ether.
  • the cellulose ether comprises one or more of methylcellulose (MC), hydroxypropylcellulose or hydroxypropylmethylcellulose (HPMC) and hydroxyethylmethylcellulose (HEMC).
  • the cellulose-based polymer comprises methylcellulose.
  • the ceramic batch mixture further comprises a lubricant component in a lubricant amount less than 1% by weight superaddition to the inorganic amount.
  • the lubricant component comprises a synthetic lubricant in an amount less than 1% by weight superaddition to the inorganic amount.
  • the lubricant component is free of synthetic lubricant.
  • the lubricant component comprises an oil lubricant.
  • the oil lubricant comprises one or more of light mineral oil, com oil, high molecular weight polybutenes, polyol esters, a blend of light mineral oil and wax emulsion, a blend of paraffin wax in com oil, and combinations of these.
  • the amount of oil lubricants is from about 1% by weight to about 10% by weight. In an exemplary embodiment, the oil lubricants are present from about 3% by weight to about 6% by weight.
  • the pore former component comprises one or more of a starch, graphite, polymer resin, or combinations thereof.
  • the ceramic batch mixture further comprises a surfactant component in a surfactant amount less than 1% by weight superaddition to the inorganic amount.
  • the surfactant component comprises one or more of C8 to C22 fatty acids, and/or their derivatives, C8 to C22 fatty esters, C8 to C22 fatty alcohols, and combinations of these.
  • the surfactant component comprises stearic, lauric, myristic, oleic, linoleic, palmitic acids, and/or their derivatives, tall oil, stearic acid in combination with ammonium lauryl sulfate, and combinations of all of these.
  • the surfactant component comprises lauric acid, stearic acid, oleic acid, tall oil, and combinations of these.
  • the amount of surfactants is from about 0.25% by weight to about 2% by weight as a super addition to the inorganic component.
  • FIG. 1 graphically illustrates wall drag curves for low, reduced, and high wall drag cordierite precursor batch mixtures, each composition containing the same inorganic component of cordierite precursor powders.
  • FIG. 2 graphically illustrates the % Strain at Break (SAB) elongation from capillary rheometer measurements for the low, reduced, and high wall drag cordierite precursor batch mixtures of FIG.1.
  • FIG. 3 graphically illustrates the wall drag Tw versus extrusion velocity (inches/second) of a high wall drag Precursor Batch Mixture for High Porosity Cordierite at 3 separate paste temperature conditions: 20 °C, 30 °C, and 40 °C.
  • FIG. 4 graphically illustrates the wall drag Tw versus extrusion velocity (inches/second) of a reduced wall drag Precursor Batch Mixture for High Porosity Cordierite, having the same inorganic component as the high wall drag mixture of FIG. 3, at 3 separate paste temperature conditions: 20 °C, 30 °C, and 40 °C.
  • FIG. 5 graphically illustrates the wall drag Tw versus extrusion velocity (inches/second) of a low wall drag Precursor Batch Mixture for High Porosity Cordierite, having the same inorganic component as the high wall drag mixture of FIG. 3 and the reduced wall drag mixture of FIG. 4, at 3 separate paste temperature conditions: 20 °C, 30 °C, and 40 °C.
  • ceramic batch mixture comprises a mixture which comprises, among other constituents, an inorganic component comprised of either ceramic constituents (e.g. cordierite or silicon carbide) or ceramic-forming precursor constituents (e.g. oxide constituents capable of being transformed into a ceramic material such as cordierite upon firing), or both.
  • the inorganic particles can comprise single-constituent particulates such as cordierite or silicon carbide, or mixtures of oxides or other compounds that are convertible to crystalline ceramic materials upon firing, such as cordierite. Ceramic products may be manufactured by employing such batch mixtures.
  • a method of manufacturing a ceramic body comprises mixing an inorganic (ceramic and/or ceramic-forming) powder component such as a cordierite and/or cordierite forming component, water as the liquid vehicle, a cellulose ether binder, and a lubricant component comprised of a fatty acid constituent and an oil constituent such as a synthetic oil constituent; the method can further comprise extruding the paste through an extrusion die, such as a honeycomb extrusion die, to produce a self-standing, or self-supporting, extrudate body.
  • the extrudate body, or a portion thereof can be fired to sinter and/or reactively sinter the extruded composition into a ceramic composition.
  • the mixture can be thoroughly blended to form a plasticized ceramic paste, and the method can further comprise pressing or extruding the ceramic paste through an extrusion die to form a self-standing body.
  • the extrusion die is a honeycomb die and the extruded self-standing body is an unfired honeycomb body that retains its extruded shape despite the presence of retained water.
  • ceramic paste comprises a paste which comprises, among other constituents, a liquid vehicle component such as water, and an inorganic component comprised of either ceramic constituents (e.g. cordierite or silicon carbide) or ceramic-forming precursor constituents (e.g. oxide constituents capable of being transformed into a ceramic material such as cordierite upon firing), or both.
  • a liquid vehicle component such as water
  • an inorganic component comprised of either ceramic constituents (e.g. cordierite or silicon carbide) or ceramic-forming precursor constituents (e.g. oxide constituents capable of being transformed into a ceramic material such as cordierite upon firing), or both.
  • the terms “unfired extruded body,” “green body,” “green ceramic body,” or “ceramic green body” refer to an non-fired body, part, or ware before firing, unless otherwise specified.
  • the terms “batch mixture,” “ceramic precursor batch,” “green composition,” and “green batch material” refer to the mixture of materials that are used to form the green body by extrusion, unless otherwise specified.
  • the non-fired extruded body and batch mixture contain a vehicle, such as water, and typically include inorganic components, and can include other materials such as binders, pore formers, lubricants, surfactants, stabilizers, plasticizers, and the like.
  • firing refers to thermal processing (heating) of the green body at an elevated temperature to form a ceramic material or a ceramic body, and comprises reaction sintering in which one or more batch materials physically react with each other to form one or more ceramic compounds, such as with cordierite-forming and aluminum- titanate forming batches, as well as sintering ceramic ingredients, such as with silicon carbide batches.
  • wt % As used herein, a “wt %,” “weight percent,” or “percent by weight” of an inorganic or organic component, unless specifically stated to the contrary, is based on the total weight of the total inorganics in which the component is included. Organic components are specified herein as super additions based upon 100% of the inorganic components used.
  • the batch mixture from which the unfired extruded body is formed includes at least one inorganic component.
  • the inorganic component may be one or more ceramic ingredient, one or more inorganic ceramic-forming ingredient, and/or combinations thereof.
  • the ceramic ingredient may be, for example, cordierite, aluminum titanate, silicon carbide, mullite, alumina, and the like.
  • the inorganic ceramic-forming ingredient may be cordieriteforming raw materials, aluminum titanate-forming raw materials, silicon carbide-forming raw materials, aluminum oxide-forming raw materials, alumina, silica, magnesia, titania, aluminum-containing ingredients, silicon-containing ingredients, titanium-containing ingredients, and the like.
  • Cordierite has the formula 2MgO.2A12O3.5SiO2.
  • the cordierite-forming raw materials may include at least one magnesium source, at least one alumina source, at least one silica source, and at least one hydrated clay.
  • sources of magnesium include, but are not limited to, magnesium oxide or other materials having low water solubility that, when fired, convert to MgO, such as Mg(OH)2, MgCO3, and combinations thereof.
  • the source of magnesium may be talc (Mg3Si4O10(OH)2), including calcined and/or uncalcined talc, and coarse and/or fine talc.
  • the at least one magnesium source may be present in an amount from about 5 wt % to about 25 wt % of the overall cordierite-forming raw materials on an oxide basis. In other embodiments, the at least one magnesium source may be present in an amount from about 10 wt % to about 20 wt % of the cordierite-forming raw materials on an oxide basis. In further embodiments, the at least one magnesium source may be present in an amount from about 11 wt % to about 17 wt %.
  • Sources of alumina include, but are not limited to, powders that, when heated to a sufficiently high temperature in the absence of other raw materials, will yield substantially pure aluminum oxide.
  • suitable alumina sources may include alpha-alumina, a transition alumina such as gamma-alumina or rho-alumina, hydrated alumina or aluminum trihydrate, gibbsite, corundum (A12O3), boehmite (A10(0H)), pseudoboehmite, aluminum hydroxide (Al(0H)3), aluminum oxyhydroxide, and mixtures thereof.
  • the at least one alumina source is a kaolin clay, and in another embodiment, the at least one alumina source is not a kaolin clay.
  • the at least one alumina source may be present in an amount from about 25 wt % to about 45 wt % of the overall cordierite-forming raw materials on an oxide basis, for example.
  • the at least one alumina source may be present in an amount from about 30 wt % to about 40 wt % of the cordierite-forming raw materials on an oxide basis.
  • the at least one alumina source may be present in an amount from about 32 wt % to about 38 wt % of the cordierite-forming raw materials on an oxide basis.
  • Silica may be present in its pure chemical state, such as a-quartz or fused silica.
  • Sources of silica may include, but are not limited to, non-crystalline silica, such as fused silica or sol-gel silica, silicone resin, low-alumina substantially alkali-free zeolite, diatomaceous silica, kaolin, and crystalline silica, such as quartz or cristobalite. Additionally, the sources of silica may further include, but are not limited to, silica-forming sources that comprise a compound that forms free silica when heated. For example, silicic acid or a silicon organometallic compound may form free silica when heated.
  • the at least one silica source may be present in an amount from about 40 wt % to about 60 wt % of the overall cordierite-forming raw materials on an oxide basis. In some embodiments, the at least one silica source may be present in an amount from about 45 wt % to about 55 wt % of the cordierite-forming raw materials on an oxide basis. In a further embodiment, the at least one silica source may be present in an amount from about 48 wt % to about 54 wt %.
  • Hydrated clays used in cordierite-forming raw materials can include, by way of example and not limitation, kaolinite (A12(Si2O5)(OH)4), halloysite (A12(Si2O5)(OH)4.H2O), pyrophylilite (A12(Si2O5)(OH)2), combinations or mixtures thereof, and the like.
  • the at least one alumina source and at least one silica source are not kaolin clays.
  • kaolin clays, raw and calcined may comprise less than 30 wt % or less than 20 wt %, of the cordierite-forming raw materials.
  • the green body may also include impurities, such as, for example, CaO, K2O, Na2O, and Fe2O3.
  • the cordierite-forming raw materials have an overall composition comprising, in weight percent on an oxide basis, 5-25 wt % MgO, 40-60 wt % SiO2, and 25-45 wt % A12O3. In other embodiments, the cordierite-forming raw materials have an overall composition comprising, in weight percent on an oxide basis, 11-17 wt % MgO, 48- 54 wt % SiO2, and 32-38 wt % A12O3.
  • the inorganic ceramic-forming ingredients can include an alumina source, a silica source, and a titania source.
  • the titania source can in one aspect be a titanium dioxide composition, such as rutile titania, anatase titania, or a combination thereof.
  • the alumina source and silica source may be selected from the sources of alumina and silica described hereinabove.
  • the amounts of the inorganic ceramic-forming ingredients are suitable to provide a sintered phase aluminum titanate ceramic composition comprising, as characterized in an oxide weight percent basis, from about 8 to about 15 wt % SiO2, from about 45 to about 53 wt % A12O3, and from about 27 to about 33 wt % TiO2.
  • an exemplary inorganic aluminum titanate precursor powder batch composition can include approximately 10% quartz; approximately 47% alumina; approximately 30% titania; and approximately 13% additional inorganic additives.
  • Additional exemplary non-limiting inorganic batch component mixtures suitable for forming aluminum titanate include those disclosed in U.S. Pat. Nos. 4,483,944; 4,855,265; 5,290,739; 6,620,751; 6,942,713; 6,849,181; 7,001,861; and 7,294,164, each of which is hereby incorporated by reference.
  • the inorganic ceramic-forming ingredients can include about 10-40%, by weight of the final batch, finely powdered silicon metal, preferably about 15-30%.
  • the silicon powder should exhibit a small mean particle size, e.g., from about 0.2 micron to 50 microns, preferably 1-30 microns.
  • the surface area of the silicon powder may, in some instances, be more descriptive than particle size, and should range between about 0.5 to 10 mSup2/Sup/g, preferably between about 1.0-5.0 mSup2/Sup/g.
  • the silicon powder is a crystalline silicon powder.
  • the silicon carbide ceramic-forming batch mixture also contains about 10-40%, by weight, of a carbon precursor, for example, a water soluble crosslinking thermoset resin having a viscosity of less than about 1000 centipoise (cp).
  • a carbon precursor for example, a water soluble crosslinking thermoset resin having a viscosity of less than about 1000 centipoise (cp).
  • the thermoset resin utilized may be a high carbon yield resin in an amount such that the resultant carbon to silicon ratio in the batch mixture is about 12:28 by weight, the stoichiometric ratio of Si — C needed for formation of silicon carbide.
  • Powdered silicon-containing fillers in an amount up to 60%, by weight, may also be included in the silicon carbide ceramic-forming batch mixture.
  • the main function of these fillers is to prevent excessive shrinkage of the green body during the carbonization and reactive consolidation/sintering steps.
  • Suitable silicon-containing fillers include silicon carbide, silicon nitride, mullite or other refractory materials. Additional exemplary nonlimiting inorganic batch component mixtures suitable for forming silicon carbide include those disclosed in U.S. Pat. Nos. 6,555,031 and 6,699,429, each of which is hereby incorporated by reference.
  • the inorganic components form an aluminum oxide ceramic
  • the inorganic components can include A12O3 and/or aluminum oxide-forming ingredients.
  • each of the batch compositions includes an organics package that may include at least a non-polar carbon chain lubricant and an organic surfactant having a polar head.
  • the organics package may also include one or more binders.
  • the organics package may also include one or more pore-forming materials.
  • the non-polar carbon chain lubricant and the organic surfactant are chemically compatible with the inorganic components, and can provide sufficient strength and stiffness to allow handling of the unfired extruded body. Additionally, the organics package is removable from the unfired extruded body during firing.
  • the batch mixtures may have an organics package in percent by weight of the inorganic components, by super addition, from about 1% to about 25% or from about 2% to about 20%. In some embodiments, the batch mixture may have an organics package in percent by weight of the inorganic components, by super addition, from about 5% to about 15%, from about 7% to about 12%, or even from about 9% to about 10%. In some embodiments, the batch mixture may have an organics package in percent by weight of the inorganic components, by super addition, from about 5% to about 11%, or about 7%.
  • Binders may include, but are not limited to, cellulose-containing components such as methylcellulose, ethylhydroxy ethylcellulose, hydroxybutyl methylcellulose, hydroxymethylcellulose, hydroxypropyl methylcellulose, hydroxyethyl methylcellulose, hydroxybutylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, sodium carboxy methylcellulose, and mixtures thereof.
  • Methylcellulose and/or methylcellulose derivatives, such as hydroxypropyl methylcellulose are especially suited as organic binders.
  • Pore-forming materials can include, for example, a starch (e.g., com, barley, bean, potato, rice, tapioca, pea, sago palm, wheat, canna, and walnut shell flour), polymers (e.g., polybutylene, polymethylpentene, polyethylene (preferably beads), polypropylene (preferably beads), polystyrene, polyamides (nylons), epoxies, ABS, acrylics, and polyesters (PET)), hydrogen peroxides, and/or resins, such as phenol resin.
  • the organic material may comprise at least one pore-forming material.
  • the organic material may comprise at least two pore-forming materials.
  • the organic material may comprise at least three pore-forming materials.
  • a combination of a polymer and a starch may be used as the pore former.
  • the non-polar carbon chain lubricant may provide fluidity to the ceramic precursor batch and may aid in the shaping of the ceramic precursor batch while also allowing the batch to remain sufficiently stiff during the forming (i.e., the extruding) process.
  • the nonpolar carbon chain lubricant can include, for example, mineral oils distilled from petroleum, synthetic and semi-synthetic base oils, including Group II and Group III paraffinic base oils, polyalphaolefins, alphaolefins, and the like. In various embodiments, the non-polar carbon chain lubricant is a polyalphaolefin.
  • Exemplary polyalphaolefins suitable for use include those sold under the trade name DURASYN®, including but not limited to DURASYN® 162 and DURASYN® 164, and SILKFLO®, including but not limited to SILKFLO® 362, available from INEOS Group AG (Switzerland), or under the trade names NEXBASE®, including but not limited to NEXBASE® 3020 (Neste Oil, Finland), and/or PARAFLEXTM, including but not limited to PARAFLEXTM HT5 (Petro-Canada, Canada).
  • the nonpolar carbon chain lubricant is present in an amount of at least 3 wt % of the inorganic components, by super addition.
  • Organic surfactants having a polar head adsorb to the inorganic particles, keeping the inorganic particles in suspension, preventing clumping, and possibly generating migration pathways.
  • the organic surfactant can include, for example, C8-C22 fatty acids and/or their ester or alcohol derivatives, such as stearic, lauric, linoleic, oleic, myristic, palmitic, and palmitoleic acids, soy lecithin, and mixtures thereof.
  • the organic surfactant is present in an amount of at least 0.3 wt % of the inorganic components, by super addition.
  • liquid vehicles such as solvents may be added to the batch mixture to create a ceramic paste (precursor or otherwise) from which the unfired extruded body is formed.
  • the solvents may include aqueous-based solvents, such as water or water-miscible solvents.
  • the liquid vehicle, or solvent is water. The amount of aqueous solvent present in the ceramic precursor batch may range from about 20 wt % to about 50 wt %.
  • a method of making a ceramic body includes adding the organics package (including at least a non-polar carbon chain lubricant and an organic surfactant) to at least one inorganic component.
  • the inorganic components and organic materials may be mixed to form a batch mixture.
  • the inorganic components may be combined as powdered materials and intimately mixed to form a substantially homogeneous powder batch.
  • the organic materials and/or solvent may be mixed with inorganic components individually, in any order, or together to form a substantially homogeneous batch.
  • Other suitable steps and conditions for combining and/or mixing inorganic components and organic materials together to produce a substantially homogeneous batch may be used.
  • the inorganic components and organic materials may be mixed by a kneading process to form a substantially homogeneous batch.
  • the batch mixture is shaped or formed into a structure using forming means, such as molding, pressing, casting, extrusion, and the like.
  • the batch mixture is extruded to form a green body. Extrusion can be achieved using, for example, a hydraulic ram extrusion press, a two stage de-airing single auger extruder, or a twin screw mixer with a die assembly attached to the discharge end of the extruder.
  • the batch mixture may be extruded at a predetermined temperature and velocity.
  • the batch mixture is formed into a honeycomb structure.
  • the honeycomb structure may include a web structure having a plurality of cells separated by cell walls.
  • each of the cell walls has a thickness of less than about 0.008 inch.
  • the reduced wall drag batch mixtures disclosed herein can be used to produce thin-walled honeycomb structures which otherwise could be susceptible to distortion resulting from, among other things, differential shear or flow of the batch mixture through the extrusion die and/or interactions between the extrusion die and the batch materials.
  • the unfired extruded body is then fired at a selected temperature under suitable atmosphere and for a time dependent upon the composition, size, and geometry of the green body to result in a fired, porous ceramic body. Firing times and temperatures depend on factors such as the composition and amount of material in the green body and the type of equipment used to fire the green body. Firing temperatures for forming cordierite may range from about 1300° C. up to about 1450° C., with holding times at the peak temperatures ranging from about 1 hour to about 8 hours and total firing times that may range from about 20 hours up to about 85 hours. Suitable firing processes may include those described in U.S. Pat. Nos. 8,187,525, 6,287,509, 6,099,793, or U.S. Pat. No. 6,537,481, each of which is incorporated by reference in its entirety.
  • Batch flow characteristics may be determined, at least in part, by the stiffness and wall drag characteristics of the ceramic paste formed from the batch.
  • the wall drag of the ceramic paste should be low enough that the ceramic paste moves through the manufacturing equipment and the extrusion dies at a reasonable pressure and with an even flow through the die.
  • fluids used to lower wall drag should not be added in quantities such that the resultant extrudate loses stiffness (e.g., slumps) or has a decrease in tensile strength.
  • the organics package of the batch mixture may be controlled to minimize wall drag while preventing slumping and retaining tensile strength, and in some embodiments even reducing the pressure used for extrusion.
  • the decreased wall drag can provide product and quality benefits, process benefits, and reductions in manufacturing costs.
  • the ability to alter the wall drag for a batch mixture may minimize bow and reduce slump, while increasing die life and reducing energy costs.
  • the batch mixtures of the various embodiments include concentrations of the non-polar carbon chain lubricant and the organic surfactant sufficient to reduce wall drag while maintaining good tensile strength and maintaining good firing characteristics.
  • the composition and/or wall drag state of the batch mixture can also affect the flow of the batch through the extruder.
  • the flow of the composition of the batch mixture may be influenced by the type of binder, the particle sizes and orientation or particles contained in the batch, and the like.
  • the flow of the batch is affected by the amount of non-polar carbon chain lubricant and the amount of organic surfactant having a polar head contained within the batch.
  • the “die life” or footage of batch through an extrusion die before recoating is needed can be a significant cost factor.
  • the rate at which products can be extruded is dependent on die pressure which includes contributions of the “wall drag” induced by the batch being forced through an extrusion die. Reduction of wall drag helps to achieve both higher rates of extrusion and longer die life.
  • Low Wall Drag (LWD) ceramic pastes may also comprise a lubricant package, such as a lubricant package of fatty acid and an oil, such as synthetic oil, such as polyalphaolefin.
  • a lubricant package such as a lubricant package of fatty acid and an oil, such as synthetic oil, such as polyalphaolefin.
  • the amounts, or ratio, of fatty acid and polyalphaolefin can vary, but while such lubricant package helps to achieve a LWD state for the paste, the lubricant package can also result in a reduced tensile characteristic of the paste.
  • the reduced tensile behavior occurs because the water content in the paste may need to be reduced in order to maintain stiffness (i.e.
  • lubricant addition may displace water), and for aqueous based pastes that comprise a cellulosic ether binder such as methylcellulose, the reduced water content or amount in the paste reduces the hydration of the methylcellulose binder responsible for achieving acceptable tensile properties.
  • aqueous based pastes that comprise a cellulosic ether binder such as methylcellulose
  • low wall drag ceramic precursor batch mixtures can provide reduced operating extrusion die pressures which can enable faster extrusion speeds/rates, can provide low die wear that can lead to longer run time on the extrusion die before the die needs to be recoated, and can allow increased stiffness leading to improved article quality
  • challenges with low wall drag batch mixtures include an increased amount of organics which are added to produce slip, which can lead to challenges in firing the extruded ware; requires increased precision for extrusion die dimensions, as reduced drag magnifies any slot to slot variability which can cause defects in the extruded ware; and can present velocity and temperature sensitivity, which can reduce tensile properties of the batch mixture.
  • high wall drag ceramic precursor batch mixtures can provide a lower required amount of lubricant, which facilitates firing; is less sensitive to extrusion die dimensions variability; although on the other hand, the high wall drag batch mixtures can require higher die operating pressure which may require slower extrusion rates; can induce high extrusion die wear; and can require a softer batch mixture in order to extrude.
  • PEO polyethylene oxide
  • methylcellulose e.g. Methocel
  • the reduced wall drag state mixture can reduce the required extrusion die pressure, for example as compared to high wall drag mixtures; can result in lower and/or slower extrusion die wear as compared to high wall drag mixtures; and exhibits velocity and temperature stability over desirable operating ranges (of temperature, speeds, etc.), i.e. the reduced wall drag state does not display velocity or temperature instability under desirable operating conditions.
  • the benefits of reduced die pressure and reduce die wear are expected to fall between those experienced for the high wall drag mixtures and the low wall drag mixtures.
  • the ratio of the amounts (in wt% with respect to the inorganic component) of the methylcellulose constituent to the polyethylene oxide is between 0.75: 1 and 1.25: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.80: 1 and 1.20: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.90: 1 and 1.10: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.95: 1 and 1.05: 1.
  • the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is about 1 : 1.
  • the batch mixture comprises methylcellulose in an amount greater than 3.0 wt% and less than 5.40 wt% with respect to the inorganic particles.
  • the cellulosic binder component is methylcellulose in an amount greater than 3.0 wt% and less than 5.40 wt% with respect to the inorganic particles.
  • a measure of tensile strength is strain at break (“SAB” or “SAB%) as measured by capillary rheometer tensile test.
  • ceramic precursor batch mixtures, or ceramic-forming pastes or ceramic pastes comprising an inorganic component comprised of inorganic particles, a cellulosic binder component, a lubricant component comprised of fatty acid and/or synthetic oil, a liquid vehicle component comprised of water, and polyethylene oxide.
  • a ratio of the amounts (in wt% with respect to the inorganic component) of the cellulosic binder component to the polyethylene oxide is between 0.5: 1 and 1.5: 1.
  • the cellulosic binder component comprises a methylcellulose constituent comprised of one or more of methylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, carboxylmethyl cellulose, and related cellulosic compounds.
  • the cellulosic binder component consists of a methylcellulose constituent.
  • the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.75: 1 and 1.25: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.80: 1 and 1.20: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.90: 1 and 1.10: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is between 0.95: 1 and 1.05: 1.
  • the ratio of the amounts (in wt%) of the methylcellulose constituent to the polyethylene oxide is about 1 : 1.
  • the batch mixture comprises methylcellulose in an amount greater than 3.0 wt% and less than 5.40 wt% with respect to the inorganic component.
  • the cellulosic binder component is methylcellulose in an amount greater than 3.0 wt% and less than 5.40 wt% with respect to the inorganic component.
  • the cellulosic binder component consists of methylcellulose.
  • the ratio of the amounts (in wt%) of the methylcellulose to the polyethylene oxide is between 0.75: 1 and 1.25: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose to the polyethylene oxide is between 0.80: 1 and 1.20: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose to the polyethylene oxide is between 0.90: 1 and 1.10: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose to the polyethylene oxide is between 0.95: 1 and 1.05: 1. In embodiments, the ratio of the amounts (in wt%) of the methylcellulose to the polyethylene oxide is about 1 : 1. In embodiments, the resulting batch mixture is in a lower wall drag state than the starting low wall drag batch mixture.
  • the PEO constituent has a molecular weight of 1 million or more. In embodiments, the PEO constituent has a molecular weight of 1-2 million. In embodiments, the PEO constituent has a molecular weight of 2 million or more. In embodiments, the PEO constituent has a molecular weight of 5 million or more. In embodiments, the PEO constituent has a molecular weight of 7 million or more.
  • the PEO constituent has a molecular weight of 5 million or less. In embodiments, the PEO constituent has a molecular weight of 4 million or less. In embodiments, the PEO constituent has a molecular weight of 3 million or less. In embodiments, the PEO constituent has a molecular weight of 2 million or less. In embodiments, the PEO constituent has a molecular weight of 1-2 million. In embodiments, the PEO constituent has a molecular weight of 1-3 million. In embodiments, the PEO constituent has a molecular weight of 1-4 million.
  • the oil constituent comprises a synthetic oil.
  • the synthetic oil comprises a polyalphaolefin.
  • the inorganic particles are comprised of cordierite precursors.
  • the batch mixture comprises methylcellulose in an amount greater than 3.0 wt% and less than 5.40 wt% with respect to the inorganic particles.
  • methods disclosed herein comprise adjusting a paste composition of a starting low wall drag ceramic and/or ceramic-forming paste or batch mixture (“starting batch mixture”), the mixture comprising an inorganic component comprised of inorganic particles, a cellulosic binder component, a lubricant component comprised of fatty acid and/or synthetic oil, and a liquid vehicle component comprised of water, the method comprising adding PEO, or increasing the amount of PEO, to the low wall drag mixture on a weight % basis with respect to the inorganic particles, and reducing the amount of the cellulosic binder component on a weight % basis with respect to the inorganic particles, such that the resulting batch mixture is in a low wall drag state.
  • starting batch mixture the mixture comprising an inorganic component comprised of inorganic particles, a cellulosic binder component, a lubricant component comprised of fatty acid and/or synthetic oil, and a liquid vehicle component comprised of water
  • the method comprising adding PEO, or increasing
  • FIG. 1 graphically illustrates wall drag curves for low, reduced, and high wall drag cordierite precursor batch mixtures, each composition containing the same inorganic component of cordierite precursor powders.
  • Each of the low, reduced, and high wall drag mixtures contained 5.40 wt% (super addition relative to the weight of the inorganic component).
  • the low wall drag composition contained 7.00 wt% polyalphaolefin synthetic oil (Durasyn) and 2.00 wt% liquid fatty acid (E213).
  • the reduced wall drag composition contained no polyalphaolefin synthetic oil, 2.00 wt% polyethylene oxide (PEO) and 0.82 wt% liquid fatty acid (E213).
  • the high wall drag composition contained 6.50 wt% polyalphaolefin synthetic oil (Durasyn) and 0.82 wt% liquid fatty acid (E213). Even with this relatively high amount of lubricant, the high wall drag composition exhibited high wall drag behavior.
  • FIG. 2 graphically illustrates the % Strain at Break (SAB) elongation from capillary rheometer measurements for the low, reduced, and high wall drag cordierite precursor batch mixtures of FIG.1.
  • SAB % Strain at Break
  • FIG. 3 graphically illustrates the wall drag Tw versus extrusion velocity (inches/second) of a high wall drag Precursor Batch Mixture for High Porosity Cordierite at 3 separate paste temperature conditions: 20 °C, 30 °C, and 40 °C, showing temperature and velocity stability in the high wall drag state.
  • FIG. 4 graphically illustrates the wall drag Tw versus extrusion velocity (inches/second) of a reduced wall drag Precursor Batch Mixture for High Porosity Cordierite, having the same inorganic component as the high wall drag mixture of FIG. 3, at 3 separate paste temperature conditions: 20 °C, 30 °C, and 40 °C, showing temperature and velocity stability in the reduced wall drag state, which are about 25 to 30 % lower than the high wall drag mixture of FIG. 3.
  • FIG. 5 graphically illustrates the wall drag Tw versus extrusion velocity (inches/second) of a low wall drag Precursor Batch Mixture for High Porosity Cordierite, having the same inorganic component as the high wall drag mixture of FIG. 3 and the reduced wall drag mixture of FIG. 4, at 3 separate paste temperature conditions: 20 °C, 30 °C, and 40 °C, showing temperature and velocity instability in the low wall drag state, with about 70% reduction compared to the high wall drag mixture of FIG. 3.

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Abstract

Production d'une pâte de précurseur de céramique de traînée de paroi réduite à l'aide de polyéthylène glycol, qui possède des propriétés entre un état de traînée de paroi faible et un état de traînée de paroi élevée.
PCT/US2023/035753 2022-10-31 2023-10-24 Procédé d'induction d'un état de traînée de paroi réduite dans une pâte de précurseur céramique à traînée de paroi élevée WO2024097048A1 (fr)

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