WO2006013931A1 - 焼成炉及びその焼成炉を用いた多孔質セラミック焼成体の製造方法 - Google Patents
焼成炉及びその焼成炉を用いた多孔質セラミック焼成体の製造方法 Download PDFInfo
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- WO2006013931A1 WO2006013931A1 PCT/JP2005/014315 JP2005014315W WO2006013931A1 WO 2006013931 A1 WO2006013931 A1 WO 2006013931A1 JP 2005014315 W JP2005014315 W JP 2005014315W WO 2006013931 A1 WO2006013931 A1 WO 2006013931A1
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- firing furnace
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Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/62—Heating elements specially adapted for furnaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/06—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity heated without contact between combustion gases and charge; electrically heated
- F27B9/062—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity heated without contact between combustion gases and charge; electrically heated electrically heated
- F27B9/063—Resistor heating, e.g. with resistors also emitting IR rays
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/14—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
- F27B9/20—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace
- F27B9/24—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace being carried by a conveyor
- F27B9/2407—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace being carried by a conveyor the conveyor being constituted by rollers (roller hearth furnace)
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/30—Details, accessories, or equipment peculiar to furnaces of these types
- F27B9/38—Arrangements of devices for charging
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/02—Ohmic resistance heating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/62—Heating elements specially adapted for furnaces
- H05B3/64—Heating elements specially adapted for furnaces using ribbon, rod, or wire heater
Definitions
- the present invention relates to a firing furnace, and more particularly to a resistance heating firing furnace for firing a ceramic material compact and a method for producing a porous ceramic fired body using the firing furnace.
- a formed body made of a ceramic raw material is fired at a relatively high temperature in a resistance heating type firing furnace.
- a resistance heating type firing furnace is disclosed in Patent Document 1. The firing furnace
- a plurality of rod heaters disposed in a firing chamber for firing the molded body.
- a material having excellent heat resistance is adopted for the resistance heating type firing furnace.
- an electric current is supplied to the rod heater to generate heat, and the molded body housed in the firing chamber is heated and sintered by the radiant heat of the rod heater to produce a ceramic sintered body. .
- Patent Document 1 JP 2002-193670 A
- a rod heater provided in a conventional resistance heating type firing furnace is formed of an extruded material.
- the material properties of the extruded material have anisotropy for manufacturing reasons. For this reason, electrical characteristics such as electrical resistance values vary widely among a plurality of rod heaters. This variation causes differences in heating characteristics such as the amount of heat generation and the temperature rise rate among the multiple rod heaters. In a firing furnace using rod heaters having different heating characteristics (quality), the furnace temperature becomes unstable or non-uniform, and it is difficult to obtain desired firing performance.
- An object of the present invention is to provide a firing furnace provided with a heating element having uniform heating characteristics, and a method for producing a porous ceramic fired body using the firing furnace.
- one embodiment of the present invention provides a firing furnace for firing an object to be fired.
- the firing furnace has a casing having a firing chamber for housing the body to be fired, and a current supply.
- a plurality of heating elements that generate heat when received and heat the object to be fired in the baking chamber.
- Each heating element is made of a material composed of crystal grains having irregular orientation.
- the present invention further provides a method for producing a porous ceramic fired body.
- the manufacturing method includes a step of forming a body to be fired from a composition containing ceramic powder, and a step of firing the body to be fired, wherein the firing step includes an enclosure having a firing chamber, and an irregular shape.
- a firing furnace including a plurality of heating elements that are formed of a material composed of crystal grains having orientation, generate heat when supplied with current, and heat the object to be fired in the firing chamber. Done.
- the material is a ceramic material formed through a cold isostatic pressing method.
- the ceramic material preferably has a porosity in the range of 5 to 20% as measured by mercury porosimetry.
- the ceramic material is carbon.
- the firing furnace of an embodiment further includes a support member that supports the plurality of heating elements, and each heating element is indirectly supported by the casing while being connected to the support member.
- the support member is preferably made of a material whose porosity measured by mercury porosimetry is adjusted in the range of 5 to 20%.
- the firing furnace can fire the object to be fired at a first temperature and a second temperature higher than the first temperature.
- the firing furnace is a continuous firing furnace that continuously fires the plurality of bodies to be fired.
- FIG. 1 is a schematic cross-sectional view of a firing furnace according to a preferred embodiment of the present invention.
- FIG. 2 is a cross-sectional view taken along line 2-2 of the firing furnace of FIG.
- FIG. 3 is an enlarged view of the electrode member of the firing furnace of FIG.
- FIG. 4 is a cross-sectional view of a cold isostatic pressing device used for forming a fired body.
- FIG. 5 is a perspective view of a particulate filter for purifying exhaust gas.
- FIGS. 6A and 6B are a perspective view and a cross-sectional view of one ceramic member for manufacturing the particulate filter of FIG.
- FIG. 1 shows a firing furnace 10 used in a ceramic product manufacturing process.
- the firing furnace 10 is provided with a housing 12 having an inlet 13a and an outlet 15a.
- the to-be-fired body 11 is carried into the housing 12 with the carry-in port 13a and is conveyed from the carry-in port 13a toward the take-out port 15a.
- the firing furnace 10 is a continuous firing furnace that continuously fires the object to be fired 11 within the housing 12. Examples of raw materials for the object to be fired are porous silicon carbide (SiC), silicon nitride (SiN), sialon, cordierite, carbon and other ceramics.
- a pretreatment chamber 13, a baking chamber 14, and a cooling chamber 15 are partitioned.
- a plurality of transport rollers 16 for transporting the object to be fired 11 are provided along the lower surfaces of the chambers 13 to 15.
- a support base l ib is placed on the transport roller 16.
- the support base l ib supports a plurality of firing jigs 11a.
- the object to be fired 11 is placed on each firing jig 11a.
- the support base l ib is pushed from the carry-in port 13a toward the take-out port 15a.
- the body 11 to be fired, the firing jig 11a, and the support base l ib are transported in the order of the pretreatment chamber 13, the firing chamber 14, and the cooling chamber 15 by the rolling of the transport roller 16.
- An example of the body to be fired 11 is a formed body formed by compressing a ceramic raw material.
- the to-be-fired body 11 is processed while moving in the housing 12 at a predetermined speed.
- the object to be fired 11 is fired when passing through the firing chamber 14.
- the ceramic powder forming the fired body 11 is sintered to obtain a sintered body.
- the sintered body is transferred to the cooling chamber 15 and cooled to a predetermined temperature.
- the cooled sintered body is taken out from the outlet 15a.
- FIG. 2 is a cross-sectional view taken along line 2-2 in FIG.
- the furnace wall 18 defines an upper surface, a lower surface, and two side surfaces of the firing chamber 14.
- the furnace wall 18 and the firing jig 11a are formed of a high heat resistant material such as carbon.
- a heat insulating layer 19 made of carbon fiber or the like is provided between the furnace wall 18 and the housing 12.
- a water cooling jacket 20 for circulating cooling water is embedded in the casing 12.
- the heat insulating layer 19 and the water cooling jacket 20 suppress the deterioration or damage of the metal parts of the casing 12 due to the heat of the firing chamber 14.
- a plurality of rod heaters (heating elements) 23 are arranged above and below the firing chamber 14, that is, so as to sandwich the body 11 to be fired in the firing chamber 14.
- each rod heater Reference numeral 23 denotes a columnar shape, and its longitudinal axis extends in the width direction of the casing 12 (the direction perpendicular to the conveying direction of the body to be fired 11).
- Each rod heater 23 is installed between both walls of the housing 12.
- the rod heaters 23 are provided in parallel to each other and at a predetermined interval.
- the rod heater 23 is entirely disposed in the firing chamber 14 from the carry-in position to the carry-out position of the body 11 to be fired.
- each rod heater 23 is electrically connected to a power source (not shown) constituting a part of the firing furnace 10 through a connector 25 and a metal electrode member 26.
- a power source (not shown) constituting a part of the firing furnace 10 through a connector 25 and a metal electrode member 26.
- Each rod heater 23 is supplied with a power source / current installed outside the housing 12 through the connector 25 and the electrode member 26.
- Each rod heater 23 generates heat during its power supply and raises the inside of the firing chamber 14 to a predetermined temperature.
- the connector 25 is formed in a cylindrical shape.
- a rod heater 23 is connected to one end of the connector 25, and an electrode member 26 is connected to the other end.
- a fixing hole 28 is formed in the side wall 12 a of the housing 12 at a position corresponding to the rod heater 23 in the firing chamber 14.
- a cup-shaped outer cylinder 29 having a bottom 29 a is attached to the fixing hole 28. The bottom 29a is exposed on the outer surface of the housing 12.
- the connector 25 is fixed to the fixing hole 30 formed in the center of the bottom 29a of the outer cylinder 29. As a result, the rod heater 23 and the electrode member 26 are stably supported.
- the connector 25 functions as a support member that indirectly supports the rod heater 23 with respect to the housing 12.
- a ring-shaped insulating member 31 is interposed between the fixing hole 30 of the outer cylinder 29 and the connector 25.
- An example of the material forming the connector 25 and the outer cylinder 29 is a high heat resistant material such as carbon.
- the ceramic material forming the rod heater 23 and the connector 25 is composed of crystal particles 32 having irregular orientation (see FIG. 3).
- the porosity of the ceramic material is preferably 5 to 20% as measured by mercury porosimetry.
- the mercury intrusion method is a method of calculating the specific surface area and pore distribution based on the pressure and the amount of mercury injected into the sample by injecting mercury into the surface and internal pores of the sample. Is the method. If the porosity of the ceramic material is less than 5%, the product yield may be lowered due to the manufacturing method. On the other hand, if the porosity of the ceramic material exceeds 20%, surface erosion due to high-temperature gas is promoted, and the rod heater 23 and the connector 25 may melt and become unusable in a short period of time. In terms of high heat resistance, it is preferred, and the ceramic material is carbon.
- the A preferred ceramic material in terms of high heat resistance, conductivity, and cacheability is graphite (graphite).
- Cortus as a raw material is pulverized to form a coatus powder having a particle size adjusted to a predetermined value.
- the preferred maximum particle size of the coatus powder is 0.02 to 0.05 mm.
- a powder composition is prepared by adding pitch as a binder to Koutus powder and kneading.
- a compact (sintered body) is produced from the powder composition.
- This molding is, for example, pressurization, and is preferably performed by a cold isostatic press method (CIP method).
- An example of pressurizing pressure for molding is about 3000 kgf / cm 2 .
- the shape of the molded body may be, for example, the shape of a force rod heater 23 or a connector 25 that is a block.
- the molded body is fired at a relatively high temperature (first temperature).
- first temperature a relatively high temperature
- second temperature a temperature higher than the first temperature
- the carbon material of the sintered body is graphitized to produce a coarse ceramic part made of a graphite material (ceramic material).
- the ceramic parts are manufactured by shaping the shape of the coarse ceramic parts.
- the first and second temperatures are about 1000 ° C and about 3000 ° C, respectively.
- Cold isostatic pressurizing device (CIP device) 40 is a pressure that accommodates a rubber mold 44 enclosing a powder composition 43, a pressurized medium (fluid) 41 such as water, and a rubber mold 44.
- a container 42 and a pump 45 for pressurizing the rubber mold 44 (and the powder composition 43) through the pressurizing medium 41 are provided.
- the pressurizing medium 41 pressurized by the pump 45 pressurizes the entire surface of the rubber mold 44 with a uniform pressure. As a result, the powder composition 43 enclosed in the rubber mold 44 is compressed with uniform pressure, and a molded body having a shape defined by the rubber mold 44 is formed.
- the porosity of the compact of the powder composition 43 can be adjusted.
- a sintered body (ceramic part) produced by firing this molded body it is easy to orient crystal grains of the ceramic material irregularly, and the porosity of the ceramic material is within the above preferred range. Easy to fit.
- the ceramic material forming the rod heater 23 and the connector 25 is made of irregularly oriented crystal particles, the characteristics of the ceramic material are isotropic.
- a resistance heating element made of such an isotropic material that is, the rod heater 23
- variation in electrical characteristics such as electrical resistance values among the rod heaters 23 is reduced, and variation in heat generation characteristics (quality). Is reduced.
- the firing furnace 10 can be heated at a uniform temperature and can exhibit a desired firing ability. Specifically, energization control of each rod heater 23 can be easily performed, and the furnace temperature in the firing chamber 14 can be easily stabilized.
- each of the plurality of rod heaters 23 can be used efficiently over a long period of time.
- the porosity of the ceramic material forming the rod heater 23 and the connector 25 is a value measured by a mercury intrusion method and is 5 to 20%.
- the number of pores exposed on the surface is reduced as much as possible.
- the entire rod heater 23 and the connection portion of the connector 25 with the rod heater 23 are constantly exposed to the high-temperature gas atmosphere in the firing chamber 14 and exposed to the surfaces of the rod heater 23 and the connector 25. Since the number of pores to be generated is small, the contact area with the gas generated in the firing chamber 14 is reduced.
- the reactivity between the rod heater 23 and the connector 25 and the high temperature gas can be kept low, and melting damage and surface erosion caused by the high temperature gas can be suppressed. Therefore, the force S can be extended to extend the service life of the rod heater 23 and the connector 25.
- the ceramic material forming the rod heater 23 and the connector 25 is formed by a cold isostatic pressing method. For this reason, the characteristics of the ceramic material are isotropic. As a result, the variation in quality regarding the electrical characteristics among the rod heaters 23 can be kept small, and it becomes easy to make the heating characteristics uniform. In the ceramic material, the number of pores exposed on the surface is reduced. As a result, melting damage and surface erosion caused by high-temperature gas are suppressed, and the service life of the rod heater 23 and the connector 25 is extended.
- the ceramic material forming the rod heater 23 and the connector 25 is excellent in heat resistance. Graphite, which is preferred from the viewpoint of carbon, is even more preferable. Thereby, the service life of the rod heater 23 and the connector 25 can be further increased.
- the firing furnace 10 is a continuous firing furnace in which the object to be fired 11 carried into the housing 12 is continuously fired in the firing chamber 14.
- the porous ceramic fired body is manufactured by forming a fired material, preparing a shaped body, and firing the formed body (fired body).
- fired materials include nitride ceramics such as aluminum nitride, silicon nitride, boron nitride and titanium nitride, carbide ceramics such as silicon carbide, zirconium carbide, titanium carbide, tantalum carbide and tungsten carbide, anolemina, Oxide ceramics such as zirconia, cordierite, mullite and silica, mixtures of multiple firing materials such as silicon and silicon carbide composites, and oxides containing multiple types of metal elements such as aluminum titanate Includes ceramics and non-oxide ceramics.
- the porous ceramic fired body is a porous non-oxide fired body having high heat, heat resistance, excellent mechanical properties, and high thermal conductivity.
- the porous ceramic fired body is a porous silicon carbide fired body.
- the porous sintered carbonized carbide is used as a ceramic member such as a particulate filter or catalyst carrier for purifying exhaust gas of an internal combustion engine such as a diesel engine.
- FIG. 5 shows a particulate filter (honeycomb structure) 50.
- the particulate finer 50 is manufactured by bundling a plurality of ceramic members 60 as a porous sintered carbide body shown in FIG. 6 (A).
- the plurality of ceramic members 60 are bonded to each other by the adhesive layer 53 to form one ceramic block 55.
- the ceramic block 55 has dimensions and shapes arranged according to the application. For example, ceramic block 55 depends on the application And is cut into a shape (cylindrical, elliptical, prismatic, etc.) according to the application.
- the side surface of the shaped ceramic block 55 is covered with a coat layer 54.
- each ceramic member 60 includes a partition wall 63 that defines a plurality of gas passages 61 extending in the longitudinal direction. At each end face of the ceramic member 60, every other opening of the gas passage 61 is closed by the sealing plug 62. That is, one opening of each gas passage 61 is closed by the sealing plug 62, and the other opening is opened.
- Exhaust gas flowing into one gas passage 61 from one end surface of the particulate filter 50 passes through the partition wall 63 and enters another gas passage 61 adjacent to the gas passage 61, and from the other end surface of the particulate filter 50. leak.
- particulate matter (PM) in the exhaust gas is captured by the partition wall 63. In this way, the purified exhaust gas flows out from the particulate filter 50.
- PM particulate matter
- the particulate filter 50 formed from the sintered carbonized carbide has extremely high heat resistance and is easy to regenerate, so that it is suitable for use in various large vehicles and vehicles equipped with diesel engines. RU
- the adhesive layer 53 for adhering the ceramic members 60 to each other may have a filter function for removing particulate matter (PM).
- the material of the adhesive layer 53 is not particularly limited, but is preferably the same as the material of the ceramic member 60.
- the coat layer 54 prevents the exhaust gas from leaking from the side surface of the particulate filter 50 when the particulate filter 50 is installed in the exhaust path of the internal combustion engine.
- the material of the coating layer 54 is not particularly limited, but is preferably the same as the material of the ceramic member 60.
- each ceramic member 60 is preferably a carbide carbide.
- the main components of each ceramic member 60 are a ceramic containing a mixture of a carbide and a metal carbide, a ceramic in which the carbide is bonded with a key or a key oxychloride, and an aluminum titanate.
- carbide ceramics other than carbide carbide, nitride ceramics, and oxide ceramics may be used.
- a preferable average pore diameter of the ceramic member 60 is 5 to: 100 x m.
- the average pore size is
- the ceramic member 60 may be clogged by the exhaust gas. If the average pore diameter exceeds 100 zm, PM in the exhaust gas may pass through the partition wall 63 of the ceramic member 60 and may not be collected by the ceramic member 60.
- the porosity of the ceramic member 60 is not particularly limited, but is preferably 40 to 80%.
- Porosity is 40. If it is less than / o, the ceramic member 60 may be clogged by the exhaust gas. If the porosity exceeds 80%, the mechanical strength of the ceramic member 60 will be low, and it will be damaged.
- a preferred firing material for producing the ceramic member 60 is ceramic particles.
- the ceramic particles preferably have a small degree of shrinkage during firing.
- a particularly preferred fired material for producing the particulate filter 50 is 100 parts by weight of relatively large ceramic particles having an average particle size of 0.3 to 50 / m, and an average of 0.1 to: 1. O xm It is a mixture of 5 to 65 parts by weight of relatively small ceramic particles having a particle size.
- the shape of the particulate filter 50 is not limited to a cylinder, and may be an elliptic cylinder or a prism.
- a fired composition material containing a carbide carbide powder (ceramic particles), a binder, and a dispersion solvent is prepared using a wet mixing and pulverizing apparatus such as an attritor.
- the fired composition is sufficiently kneaded with a kneader, and formed into a formed body (fired body 11) having the shape (hollow prism) of the ceramic member 60 in FIG. 6 (A) by, for example, extrusion molding.
- the type of the binder is not particularly limited, but methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyethylene glycol, phenol resin, and epoxy resin are generally used.
- the preferred amount of Noinda is 1 to 10 parts by weight with respect to 100 parts by weight of the carbide carbide powder.
- the type of the dispersion solvent is not particularly limited, but a water-insoluble organic solvent such as benzene, a water-soluble organic solvent such as methanol, and water are generally used.
- the preferred amount of the dispersion solvent is determined so that the viscosity of the fired composition is within the integral range.
- the body to be fired 11 is dried. If necessary, seal one opening of some gas passages 61
- a plurality of dried objects to be fired 11 are placed side by side on the firing jig 11a.
- a plurality of firing jigs 11a are stacked and placed on the support base l ib.
- the support table l ib is moved by the conveying roller 16 and passes through the baking chamber 14. At this time, the body 11 to be fired is fired to produce a porous ceramic member 60.
- a plurality of ceramic members 60 are bonded to each other by an adhesive layer 53 to form a ceramic filter block 55. Adjust the dimensions and shape of the ceramic block 55 according to the application. A coat layer 54 is formed on the side surface of the ceramic block 55. In this way, the particulate filter 50 is completed.
- a rod heater 23 was formed from a carbon material (hereinafter referred to as CIP material) manufactured by a cold isostatic pressing method (CIP method).
- CIP method cold isostatic pressing method
- the rod heater 23 was formed from a carbon material (extruded material) manufactured by an extrusion method.
- Each rod heater 23 was placed in the firing furnace 10, and the voltage drop time (hr) of each rod heater 23 was measured by supplying a current and causing resistance heating. The longer the voltage drop time, the longer the service life.
- the furnace atmosphere of the firing furnace 10 is an argon (Ar) atmosphere, and the furnace temperature is about 2200 ° C.
- Table 1 shows the evaluation results and various physical properties of the carbon materials used in Examples:! -3 and Comparative Examples:! -3.
- the voltage drop time of Examples:! To 3 is more than twice that of Comparative Examples:! To 3, and the rod heaters of Examples 1 to 3 have a longer service life.
- the reason is presumed as follows.
- the comparative heater 23 is susceptible to melting and surface erosion due to high-temperature gas due to the numerous pores exposed on the surface.
- the rod heater 23 of the example since there are few pores exposed on the surface, the rod heater 23 is less susceptible to melting damage and surface erosion due to high temperature gas.
- the molded body was subjected to primary drying at 100 ° C for 3 minutes using a microwave dryer. Subsequently, the compact was subjected to secondary drying at 110 ° C. for 20 minutes using a hot air dryer.
- the dried molded body was cut to expose the open end face of the gas passage.
- Sealing plugs 62 were formed by filling the openings of some gas passages with carbon carbide paste.
- the support base l ib on which the plurality of molded bodies 11 were placed was carried into a continuous degreasing furnace.
- the compact 11 was degreased by heating at 300 ° C in a mixed gas atmosphere of air and nitrogen with the oxygen concentration adjusted to 8%.
- the support base l ib was carried into the continuous firing furnace 10.
- a square pillar-shaped porous silicon carbide fired body (ceramic member 60) was produced by firing at 2200 ° C. for 3 hours under an atmospheric pressure argon gas atmosphere.
- alumina fiber having a fiber length of 20 ⁇ m 30% by weight of alumina fiber having a fiber length of 20 ⁇ m, 20% by weight of carbon carbide particles having an average particle diameter of 0.6 ⁇ m, 15% by weight of silica sol, 5.6
- An adhesive paste containing 2% by weight and 28.4% by weight of water was prepared. This adhesive paste is heat resistant.
- a ceramic block 55 was formed by bonding 16 ceramic members 60 to a 4 ⁇ 4 bundle with this adhesive paste. The shape of the ceramic block 55 was adjusted by cutting and cutting the ceramic block 55 with a diamond cutter.
- An example of the ceramic block 55 is a cylinder having a diameter of 144 mm and a length of 150 mm.
- Inorganic fiber (ceramic fiber like alumina silicate, fiber length 5 ⁇ : 100 ⁇ m, shot content 3%) 23.3% by weight, inorganic particles (carbon carbide particles, average particle size is 0.3 xm) 30.2% by weight, inorganic binder (containing 30% Si02 in the sol) 7% by weight, organic binder (carboxymethylcellulose) 0.5% by weight, water 39% % Were mixed and kneaded to prepare a coating material paste.
- the particulate filter 50 of Example 4 satisfies various characteristics required for an exhaust gas purification filter. Since the plurality of ceramic members 60 are continuously fired in the firing furnace 10 at a uniform temperature, characteristics such as pore diameter, porosity, and mechanical strength are reduced from being dispersed among the ceramic members 60, and the Variations in the characteristics of the curate filter 50 are also reduced.
- the firing furnace of the present invention is suitable for manufacturing a porous ceramic fired body.
- the cold isostatic pressurization method is a dry method in which the pressure is applied through the rubber mold incorporated in the pressure vessel 42, which was a wet method in which the rubber mold 44 is immersed in the pressurizing medium 41 and pressurized. It may be changed.
- Rod heater 23 may be formed of a silicon carbide ceramic material.
- the rod heater 23 and the connector 25 may be integrally formed.
- the shape of the heating element may be other than a cylinder, for example, a flat plate, a square bar, or a square.
- the shape of the body to be fired 11 is arbitrary.
- the firing furnace 10 may be other than a continuous firing furnace, for example, a batch-type firing furnace.
- the firing furnace 10 may be used outside the ceramic product manufacturing process, for example, a heat treatment furnace used in a semiconductor or electronic component manufacturing process, a reflow furnace, or the like. Good.
- the particulate filter 50 includes a plurality of filter elements 60 bonded to each other by an adhesive layer 53 (adhesive paste).
- One filter element 60 may be used as the palate rate filter 50.
- the coating layer 54 (coating material paste) may or may not be applied to the side surface of each filter element 60.
- Ceramic fired body is suitable for use as a catalyst carrier.
- the catalyst are noble metals, alkali metals, alkaline earth metals, oxides, and combinations of two or more thereof, but the type of catalyst is not particularly limited. Platinum, palladium, rhodium or the like can be used as the noble metal.
- As the alkali metal, potassium, sodium, etc. can be used. Barium or the like can be used as the alkaline earth metal.
- oxides include perovskite oxides (La K MnO, etc.), CeO, etc.
- the ceramic fired body supporting such a catalyst is not particularly limited, and can be used as, for example, a so-called three-way catalyst or NOx storage catalyst for automobile exhaust gas purification.
- the catalyst may be supported on the fired body after the ceramic fired body is created, or may be supported on the raw material (inorganic particles) of the fired body before the fired body is created.
- An example of a catalyst loading method is an impregnation method, but there is no particular limitation.
Abstract
Description
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Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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JP2006531549A JPWO2006013931A1 (ja) | 2004-08-04 | 2005-08-04 | 焼成炉及びその焼成炉を用いた多孔質セラミック焼成体の製造方法 |
EP05768496A EP1818639A4 (en) | 2004-08-04 | 2005-08-04 | FURNACE AND METHOD FOR PRODUCING A BURNTED POROUS CERAMIC ARTICLE USING THE FUEL |
US11/312,488 US20060118546A1 (en) | 2004-08-04 | 2005-12-21 | Firing furnace and method for manufacturing porous ceramic fired object with firing furnace |
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JP2004-228571 | 2004-08-04 | ||
JP2004228571 | 2004-08-04 |
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US11/312,488 Continuation US20060118546A1 (en) | 2004-08-04 | 2005-12-21 | Firing furnace and method for manufacturing porous ceramic fired object with firing furnace |
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US (1) | US20060118546A1 (ja) |
EP (1) | EP1818639A4 (ja) |
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Cited By (3)
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JP2008175517A (ja) * | 2006-03-08 | 2008-07-31 | Ibiden Co Ltd | 焼成体用冷却機、焼成炉、セラミック焼成体の冷却方法、及び、ハニカム構造体の製造方法 |
EP2953421A1 (en) | 2014-06-03 | 2015-12-09 | Ibiden Co., Ltd. | Carbon heater, heater unit, firing furnace, and method for manufacturing silicon-containing porous ceramic fired body |
JP2015230766A (ja) * | 2014-06-03 | 2015-12-21 | イビデン株式会社 | カーボンヒータ、ヒータユニット、焼成炉及び珪素含有多孔質セラミック焼成体の製造方法 |
Also Published As
Publication number | Publication date |
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EP1818639A1 (en) | 2007-08-15 |
US20060118546A1 (en) | 2006-06-08 |
JPWO2006013931A1 (ja) | 2008-05-01 |
EP1818639A4 (en) | 2007-08-29 |
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