WO2004035281A1 - セラミック成形体の製造方法 - Google Patents
セラミック成形体の製造方法 Download PDFInfo
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- WO2004035281A1 WO2004035281A1 PCT/JP2003/013163 JP0313163W WO2004035281A1 WO 2004035281 A1 WO2004035281 A1 WO 2004035281A1 JP 0313163 W JP0313163 W JP 0313163W WO 2004035281 A1 WO2004035281 A1 WO 2004035281A1
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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
- C04B35/10—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 aluminium oxide
- C04B35/111—Fine ceramics
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- 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
- B28B13/00—Feeding the unshaped material to moulds or apparatus for producing shaped articles; Discharging shaped articles from such moulds or apparatus
- B28B13/04—Discharging the shaped articles
- B28B13/06—Removing the shaped articles from moulds
- B28B13/065—Removing the shaped articles from moulds by applying electric current or other means of discharging, e.g. pneumatic or hydraulic discharging means
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- 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
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/34—Moulds, cores, or mandrels of special material, e.g. destructible materials
- B28B7/342—Moulds, cores, or mandrels of special material, e.g. destructible materials which are at least partially destroyed, e.g. broken, molten, before demoulding; Moulding surfaces or spaces shaped by, or in, the ground, or sand or soil, whether bound or not; Cores consisting at least mainly of sand or soil, whether bound or not
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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
- C04B35/624—Sol-gel processing
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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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- 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
- C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
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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
- C04B35/6264—Mixing media, e.g. organic solvents
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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
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
- H01J9/245—Manufacture or joining of vessels, leading-in conductors or bases specially adapted for gas discharge tubes or lamps
- H01J9/247—Manufacture or joining of vessels, leading-in conductors or bases specially adapted for gas discharge tubes or lamps specially adapted for gas-discharge lamps
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6023—Gel casting
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/94—Products characterised by their shape
Definitions
- the present invention relates to a method for manufacturing a ceramic molded body. Background technology
- a ceramic slurry containing a ceramic powder, a dispersion medium and a gel agent is molded in a molding die, and the molded body is released from the molding die to form a ceramic.
- the manufacturing method of this method is a so-called gel casting method.
- the method of manufacturing a ceramic molded body proposed in each of the above-mentioned patent documents is a gel cast method using a special ceramic slurry as a ceramic slurry for molding, and a ceramic having a complicated shape and structure. It is adopted as a material suitable for forming a molded body with high dimensional accuracy.
- a ceramic molded body of this method it is possible to form a ceramic molded body having a complicated shape and structure with high dimensional accuracy.
- the presence of slight damage, such as cracks, is not allowed. Even if there is a slight damage to the ceramic compact, this slight damage will adversely affect the mechanical and thermal strength of the ceramic compact.
- the ceramic molded body is fired to be a product as a sintered body, slight damage is a major cause of damage during firing, and the ceramic molded body is a sintered body. It may not be possible to manufacture a product.
- an outer mold made of a non-soluble material and a soluble mold that is housed in the outer mold and forms a predetermined cavity inside the outer mold are used as a molding die.
- a mold having a core made of a material is employed. In the mold, a molded body is produced with the core built-in. For this reason, when releasing the molded article, the molded article must be released from both the outer mold and the core.
- a wax core that is easy to melt at a low temperature is used as the core.
- Means are employed for thermally melting the core in the body and discharging the molten state from the molded body. In this mold release means, the thermal expansion force of the core at the time of thermal melting acts on the molded body, and there is a fear that the molded body may be damaged such as cracks. Disclosure of the invention
- an object of the present invention is to prevent a molded article from being slightly damaged, such as a crack, in the method for producing each ceramic article employing the production method of the method. Furthermore, a main object of the present invention is to provide a molded article that has a small shrinkage during molding and does not cause damage such as cracks due to shrinkage during molding, and that is difficult to release from a mold. Another object of the present invention is to prevent the occurrence of damage to a molded article during mold release by smoothly releasing the mold from the molding die without any resistance.
- a first method for producing a ceramic molded body according to the present invention is a method for producing a solid ceramic molded body, comprising forming a ceramic slurry containing ceramic powder, a dispersion medium and a gel agent in a molding die. And a method for producing a ceramic molded body by releasing the molded solid molded body from the molding die to obtain a ceramic molded body.
- the solid molded body in the mold is heated to melt the solid contained in the molded body.
- the agent is extracted to the outside of the molded article, and thereafter, the solid molded article is released from the mold.
- a second method for producing a ceramic molded body according to the present invention is a method for producing a hollow ceramic molded body having a cavity therein, and comprises a ceramic powder, a dispersion medium, and a gelling agent. This is a method for producing a ceramic molded body in which a rally is molded in a mold, and the molded hollow molded body is released from the mold to obtain a hollow ceramic molded body.
- an outer die made of a non-soluble material, and a predetermined cavity housed in the outer die together with the outer die are provided.
- a mold having a core made of a soluble material to be formed is employed, and the ceramic slurry is injected into the cavity in the mold to form a hollow molded body having a cavity therein.
- the hollow molded body in the outer mold is heated, and the solvent contained in the hollow molded body is discharged to the outside of the hollow molded body. Extracting, and then releasing the hollow molded body from the outer mold.
- a core made of a heat-fusible material can be adopted as a core constituting the molding die.
- the core of the hollow molded body from the outer die is used.
- the hollow molded body in the mold is heated to extract the solvent contained in the hollow molded body to the outside of the hollow molded body, and the solvent existing in the hollow molded body is extracted.
- the melt is melted and discharged from the hollow molded body. Thereafter, the hollow molded body is released from the outer mold.
- the ceramic slurry used for molding the ceramic molded body may be a ceramic slurry having a body shrinkage of 5% or less in the molding die. Is preferably selected.
- the molded body in the molded mold is heated when the molded body is released from the mold.
- the solvent existing in the pores of the molded body expands and is extracted to the outside of the molded body, and the extracted solvent is formed between the outer peripheral surface of the molded body and the inner peripheral surface of the molding die.
- a solvent film forms between them.
- the molded body has no resistance due to the action of the solvent film.
- the mold can be released from the mold, and it is possible to prevent the molded body from being damaged due to resistance from the mold at the time of release.
- the mold release means in the first manufacturing method according to the present invention is a mold release method for a solid molded body which has no shrinkage in the mold or is extremely small and does not generate any damage such as slight cracks. Mold release. This makes it possible to produce a ceramic molded body having high mechanical strength and thermal strength without causing damage such as cracks due to shrinkage in the mold.
- the mold release means in the second production method according to the present invention is also the most suitable means for releasing the hollow ceramic molded body from the outer mold for the same reason as described above.
- means for releasing the hollow molded body from the core by discharging the core existing in the hollow molded body from the molded body in a molten state can be employed.
- the release means is performed in a state where the molded body is in the outer mold.
- the core thermally expands during the heating and melting, and the thermal expansion force acts in the hollow of the hollow molded body.
- the hollow molded body is released from the outer mold, the hollow molded body is likely to be damaged by the acting force.
- the core is heated and melted and discharged in a molten state while the hollow molded body is in the outer mold, the working force due to thermal expansion is reduced. As a result, it is possible to prevent the hollow molded body from being damaged due to the acting force.
- the contained solvent forms not only the outer peripheral surface side of the hollow molded body but also a cavity.
- the solvent film is also formed between the inner peripheral surface of the hollow molded body and the outer peripheral surface of the core by extracting on the inner peripheral surface side. This solvent film regulates the intrusion of a molten substance such as a molten box into the pores in the hollow molded body when the core is melted.
- the body shrinkage is preferably 5% or less. It is necessary to mold the compact.
- the molded body can be molded by selecting a ceramic slurry for molding. And, as a solvent contained in the ceramic slurry, its body expansion coefficient is
- FIG. 1 is a process diagram showing a general manufacturing process for manufacturing a hollow ceramic molded article according to the present invention and a light emitting container using the same as a precursor.
- FIG. 2 is a process chart showing a general manufacturing process for manufacturing a solid ceramic molded body according to the present invention and a container using the same as a precursor.
- FIGS. 3A to 3C are schematic diagrams (a) to (c) schematically showing each manufacturing process in a manufacturing experiment using the method for manufacturing a hollow ceramic molded body according to the present invention.
- Fig. 4 is a schematic diagram (a) schematically showing the step of discharging the plastic molded body in a molten state in the same production experiment, and (b) a schematic diagram showing the outline of the hollow ceramic molded body released from the mold. .
- a first method of manufacturing a ceramic molded body according to the present invention comprises molding a ceramic slurry containing a ceramic powder, a dispersion medium, and a gelling agent in a molding die, and molding the molded solid molded body into the same molding die.
- This is a method for producing a ceramic molded body that is released from a mold to obtain a solid ceramic molded body.
- the solid molded body in the molded mold is heated to extract the solvent contained in the solid molded body to the outside of the molded body. Thereafter, means for releasing the solid molded body from the molding die is adopted.
- a second method for producing a ceramic molded body according to the present invention includes: A method for producing a ceramic molded body in which a ceramic slurry containing a dispersion medium and a gelling agent is molded in a molding die, and the molded hollow molded body is released from the molding die to obtain a hollow ceramic molded body. It is.
- As the mold an outer mold made of an insoluble material and a mold having a core made of a soluble material housed in the outer mold and forming a predetermined cavity with the outer mold are employed.
- a ceramic slurry is injected into a cavity in a mold to obtain a hollow ceramic molded body having a cavity therein.
- the hollow molded body in the outer mold of the molded mold is heated to extract the solvent contained in the hollow molded body to the outside of the hollow molded body. Thereafter, means for releasing the hollow molded body from the outer mold is adopted.
- the manufacturing method based on the manufacturing process shown in FIG. 1 is employed in the manufacturing method of the hollow ceramic molded body.
- a manufacturing method based on the manufacturing process shown in FIG. 2 is employed.
- a ceramic slurry that is a molding slurry and has a body shrinkage of 5% or less in the molding die during molding is selected, and the molding die of the molded body is formed during molding.
- the purpose of the present invention is to produce a ceramic molded body that does not cause damage such as cracks due to shrinkage in the inside.
- the molded body has a large resistance to the mold at the time of release from the mold, and is easily damaged.
- the mold release means that can be released and does not cause damage to the molded body is adopted.
- the second manufacturing method according to the present invention for manufacturing a hollow ceramic molded body it is very difficult to release the hollow ceramic molded body from the core, and the hollow ceramic molded body is released without being damaged. Is not easy. For this reason, in order to facilitate mold release, a core made of wax that melts at a low temperature is used as the molding material, and the core built in the hollow ceramic molded body is heated and melted, and the hollow ceramic is melted. Means for discharging from the molded body are adopted.
- the hollow ceramic molded body in the outer mold is heated to remove the solvent contained in the hollow ceramic molded body from the hollow ceramic molded body. It is extracted to the outside of the molded body, and then the core of the hollow ceramic molded body is heated and melted and discharged from the hollow ceramic molded body in a molten state. Next, the hollow ceramic molded body is released from the outer mold.
- the preferred ceramic slurry employed in each of the production methods according to the present invention comprises a ceramic powder as a raw material powder, a dispersion medium and a gelling agent as main constituent components. It is preferable to select a ceramic slurry that has a body shrinkage of 5% or less in the mold. To cope with this, it is necessary to select the solvent that will be included with each component when preparing the ceramic slurry.
- the solvent the body expansion coefficient, 0. 5 0 X 1 0- 3 ZK ⁇ 2. 0 X 1 CT 3 / K, preferably 1. 0 0 X 1 0- 3 ! ⁇ ⁇ 1.
- the dispersion medium and the gelling agent contain an organic compound having a reactive functional group, and these organic compounds can react with each other.
- the curing efficiency is high in ceramic rallies, and due to the high curing efficiency, desired curing characteristics can be obtained by adding a small amount of a gelling agent.
- the ceramic slurry can be kept low in viscosity and high in fluidity.
- the above-mentioned reactive functional group means an atomic group or a molecular group capable of chemically reacting with other components, such as a hydroxyl group, a carbonyl group, a carbonyl group, an amino group, a carbonyl group formed by an ester bond described later, A methoxy group and the like can be mentioned.
- Organic compounds contained in the dispersion medium include, among organic compounds having a reactive functional group, esters such as low-viscosity liquid substances having a viscosity at 20 ° C. of 20 cps or less. preferable. Particularly, esters having a total carbon number of 20 or less are preferable. Further, the ester bond preferably has a CH 3 —O—CO— group. Esters are relatively stable, but by using a highly reactive gelling agent, the reactivity of the entire slurry can be increased.
- the organic compound constituting the dispersion medium may have one reactive functional group.However, in order to exhibit a higher gelling ability and sufficiently cure the ceramic slurry, two or more reactive functional groups are required. Organic compounds having a group are preferred. Examples of the organic compound having two or more reactive functional groups include diols such as ethylene glycol; polyhydric alcohols such as triols such as glycerin; polybasic acids such as dicarboxylic acid; dimethyl dartrate; and malonic acid. Esters such as polybasic acid esters such as dimethyl, triacetin and the like, esters of polyhydric alcohols and the like can be mentioned.
- the organic compound that constitutes the dispersion medium achieves a high reaction rate to sufficiently cure the ceramic slurry, and imparts high fluidity to the ceramic slurry before curing to form high-density and precise molded products.
- Esters having two or more ester bonds such as polybasic acid esters such as dimethyl dallate, and acid esters of polyhydric alcohols such as triacetin are preferred.
- the reactive functional groups in the molecule do not necessarily need to be the same kind of functional group, and may be different kinds of functional groups. However, for the reasons described above, it is preferable that the compound contains at least one ester bond. Further, the dispersion medium does not necessarily need to be composed only of an organic compound having a reactive functional group, and may contain a non-reactive component.
- Acceptable non-reactive components include, for example, ethers, hydrocarbons, toluene, and the like. These non-reactive components may be selected according to chemical properties such as compatibility with an organic compound having a reactive functional group constituting a dispersion medium and a dispersant described below. For example, when an ester is used as the organic compound having a reactive functional group constituting the dispersion medium, it is preferable to contain an ether from the viewpoint of compatibility and the like. Even when an organic compound is used as a non-reactive component, in order to ensure sufficient reaction efficiency with the gelling agent, an organic compound having a reactive functional group is required to be 60 mass% in the entire dispersion medium. % Is preferable. More preferably, It is at least 85% by mass.
- the gelling agent forming the ceramic slurry contains an organic compound having a reactive functional group, which reacts with an organic compound having a reactive functional group which forms a dispersion medium to cure the ceramic slurry.
- the organic compound constituting the gelling agent may be any organic compound having a reactive functional group which chemically reacts with the organic compound in the dispersion medium in the molecule. Examples of such an organic compound include monomers, oligomers, prepolymers that are three-dimensionally crosslinked by the presence of a crosslinking agent, such as polyvinyl alcohol, epoxy resin, and phenol resin.
- the organic compound constituting the gelling agent is preferably one having a low viscosity from the viewpoint of ensuring the fluidity of the ceramic slurry, specifically, a liquid substance having a viscosity at 20 at 30 cps or less.
- a low-viscosity organic compound a compound having a molecular weight smaller than that of a polymer or a prepolymer, specifically, a monomer or oligomer having an average molecular weight (by the GPC method) of 200 MW or less is preferable.
- the viscosity means the viscosity of the organic compound having a reactive functional group constituting the gelling agent itself, and the viscosity of the organic compound diluted with a diluent such as an aqueous solution. Not something.
- the gelling agent may be one in which such an organic compound having a reactive functional group is dispersed or dissolved in a diluent, but as described above, the organic compound contributing to the reaction itself has a low viscosity. Since the reaction efficiency can be increased, dilution with a diluent is not necessary, and when a diluent is used, it is preferable to use the diluent only to a minimum amount necessary for obtaining a predetermined viscosity.
- the organic compound constituting the gelling agent it is preferable to select an organic compound having a suitable reactive functional group in consideration of the reactivity with the organic compound in the dispersion medium.
- isocyanates are generally reacted with diols and diamines, but dials are often highly viscous and diamines are highly reactive. Care should be taken because the slurry may harden before it is poured into the mold.
- Chemical substances based on the chemical structure represented by the general formula (1) are 4, 4'-diphenyl methane diisocyanate isocyanate (resin)-MD I isocyanate
- the chemical substance based on the chemical structure represented by the general formula (2) is a hexamethylene diisocyanate-based isocyanate (resin) -HD I-based isocyanate, and based on the chemical structure represented by the general formula (3)
- the chemical substance is tolylene diisocyanate isocyanate (resin) to TDI isocyanate.
- the chemical substance having the chemical structure represented by the general formula (4) is isophorone diisocyanate isocyanate.
- (Resin) DI isocyanate, a chemical substance based on the chemical structure represented by the general formula (5) is isothiocyanate (resin).
- HD I-based isocyanates (resins) based on the chemical structure represented by the general formula (2) are based on the chemical structures represented by the following general formulas (6) to (8). Dimer or trimer.
- the organic compound constituting the gelling agent is preferably an MDI-based isocyanate (resin) or an HDI-based isocyanate (resin), more preferably an MDI-based isocyanate (resin).
- these isocyanates (resins) are used as the gelling agent, they are formed.
- the hardness of the molded body is improved, and the occurrence of cracks can be suppressed even if the molded body has a thin structure.
- shrinkage of the formed compact during drying is reduced, it is possible to suppress the occurrence and deformation of cracks during drying of the compact.
- the curing speed of the slurry during the formation of the molded body is improved, and the molding process can be sped up.
- the gelling agent other functional groups can be introduced into each of the above basic chemical structures in consideration of chemical properties such as compatibility with a dispersion medium and the like.
- compatibility with the ester is increased to improve the compatibility.
- a reactive functional group other than an isocyanate group or an isothiocyanate group can be contained in the molecule of the organic compound constituting the gelling agent. In this case, an isocyanate group / isothiocyanate group may be mixed, and a large number of isocyanate group / isothiocyanate group may be present like a polyisocyanate group.
- the gelling agent constituting the ceramic slurry greatly affects the shrinkage of the molded body in the mold, and the gelling agent having the structure represented by the above general formulas (1) and (2) is A ceramic slurry for a compact having a small body shrinkage is formed, and the gelling agent having the structure represented by the general formulas (3) to (5) is followed by the gelling agent having the structure represented by the general formulas (6) to (5).
- the gelling agent having the structure shown in (8) constitutes a ceramic slurry for a compact having a relatively large body shrinkage.
- the structure represented by the above general formulas (1) and (2) must be used. It is necessary to employ a gelling agent. It is preferable that the ceramic slurry does not harden when injected into the mold, but quickly hardens in the mold after the injection. Therefore, when preparing the ceramic slurry, the temperature of the slurry before injection, the type and content of the reactive dispersion medium, the type and content of the reactive gelling agent, and the presence or absence of a catalyst that contributes to the gelation reaction It is preferable to consider the type and content of the catalyst.
- the raw material powder ceramic powder may be added to the dispersion medium and dispersed, and then the gelling agent may be added and dispersed.
- the ceramic powder and the gelling agent may be simultaneously dispersed in the dispersion medium. It can also be added to and dispersed.
- the slurry viscosity of the ceramic slurry at 20 ° C. is preferably 300 cps or less, more preferably, the slurry viscosity at 2 O: It is less than 200 cps.
- the slurry viscosity in 25: is preferably 5 cps or less.
- the slurry concentration (volume% of raw material powder with respect to the total volume of the slurry) is low. In the case of too small, the density of the slurry is 25% because the density of the formed ceramic body is reduced and the strength of the formed body is reduced, and cracks and deformation are apt to occur during drying and firing of the formed body. % By volume to 75% by volume, preferably from 35% by volume to 75% by volume. The viscosity of the slurry is adjusted by the concentration of the slurry, the viscosity of the reactive dispersant and the gelling agent, the type of the ceramic powder, and the amount of other additives added as necessary.
- molding die In the method of manufacturing a solid ceramic molded body, an ordinary split-type metal molding die is used as the molding die used in the production of the ceramic molded body according to the present invention. In the molding die, the inner peripheral surface of each die forming the cavity is extremely smooth.
- a mold having a split type outer mold and a core arranged in the outer mold and forming a cavity between the inner mold and an inner peripheral surface thereof is provided.
- the inner peripheral surface forming the outer cavity is extremely smooth, and the outer peripheral surface forming the core cavity is extremely smooth.
- the mold is, for example, one shown in FIGS.
- FIG. 3 shows an embodiment for producing a hollow ceramic molded body according to the present invention, and FIG. 3 shows the separation of the hollow ceramic molded body with respect to a core employed in the embodiment. It shows a mold means.
- the molding die 10 used in this embodiment is a split type outer die 11 composed of a pair of split dies 1 la and 11 b and a core 12, which constitutes the outer die 11.
- Each of the split dies 11a and 11b is made of stainless steel, and the core 12 is composed of a wax molded body 12a and pins 12b.
- the ceramic slurry was injected from the injection port 11 of the outer die 11 to the cavity 13 formed by the inner peripheral surface of the outer die 11 and the outer peripheral surface of the core 12.
- the hollow ceramic molded body 20 is formed by gelling and hardening the ceramic slurry that has been injected and injected.
- the molded hollow ceramic molded body 20 is released from the inside of each of the divided molds 11 a and 11 b of the outer mold 11 by dividing the outer mold 11.
- the wax molded body 12 a constituting the core 12 is discharged from the hollow ceramic molded body 20 in a heated and molten state.
- the core 12 constituting the mold 10 for the hollow molded body is integrated with the outer mold 11 It forms a hollow portion of a hollow ceramic molded body, and has a molded body 12 a and a pin 12 b corresponding to the shape of the hollow portion.
- One form of the core 12 is formed by penetrating a pin 12b at the center of a wax molded body 12a.
- the melting point is in the range of 30 ° (: to 8 O :), and the viscosity of the wax at the time of melting is 10 cps or less. It is preferable that the volume change rate due to the phase transition of the melt-solidification of the wax is 5% or less, etc.
- the pin 12 b constituting the core 12 is A configuration in which the wax molded body 12a is penetrated and joined to the wax molded body 12a can be employed, but instead of such a configuration, the pin 12b is planted in the wax molded body 12a.
- the pin 12b itself may be any of a solid pin and a tubular hollow pin.
- the first production method according to the present invention is a method for producing a solid ceramic molded body
- the second production method according to the present invention is a method for producing a hollow ceramic molded body.
- Each of these manufacturing methods is a gel cast method in which each of the above-mentioned ceramic slurries and each of the molding dies are selected and used. In both of the production methods, a large method is particularly required for releasing the molded product from the molding die. It has features.
- Fig. 1 is a flow chart showing each manufacturing process in a general manufacturing method of a hollow ceramic molded body
- Fig. 2 is a flowchart showing each manufacturing process in a general manufacturing method of a solid ceramic molded body. is there.
- a hollow ceramic molded article or a solid ceramic molded article is molded using a ceramic slurry, and the molded hollow ceramic molded article or solid ceramic molded article is formed. These are used as precursors and are fired to produce hollow ceramic parts or solid ceramic parts, which are products of sintered bodies.
- hollow ceramic molded bodies In the production of hollow ceramic molded bodies, it is intended to form a hollow ceramic molded body and then sinter it to produce a light-emitting container (hollow ceramic part) as a sintered body.
- the hollow ceramic component has a hollow ceramic molded body as a precursor.
- a light-emitting container for a high-pressure discharge lamp In the production of a solid ceramic molded body, for example, a simple bowl-shaped solid ceramic molded body that opens upward is fired, and then sintered into various bowl-shaped solid ceramic parts. It is intended to be manufactured.
- the solid ceramic component is a bowl-shaped container using a solid ceramic molded body as a precursor.
- Figure 1 shows the manufacturing process from the preparation of a ceramic slurry, which is a molding slurry, to the production of a hollow ceramic molded body, and the production of a light emitting container using the hollow ceramic molded body as a precursor.
- These manufacturing steps are general manufacturing steps in the manufacturing method according to the present invention, and include a step of preparing a molding slurry, a step of forming a hollow ceramic formed body, a step of releasing a hollow ceramic formed body, and a step of forming a hollow ceramic. It comprises a calcining and firing step of the molded body, and the luminous container is manufactured in the order of these steps.
- the step of preparing the forming slurry is to prepare a ceramic slurry which is a forming slurry of the hollow ceramic formed body.
- the ceramic powder, the dispersion medium, and the dispersant are mixed with each other to prepare a slurry, and the prepared slurry is disintegrated. Thereafter, a gelling agent, a reaction catalyst, etc. are added to make a final preparation of the slurry, and the slurry is defoamed before being poured into a mold.
- Crushing in the preparation process of the molding slurry is performed by a pot mill, a pole mill, or the like, and is performed at a temperature of 15 ° C to 35 for 96 hours, preferably 120 hours or more using a Nihon boulder. .
- the defoaming of the slurry is performed by stirring the slurry in a vacuum atmosphere, and a vacuum of -0.09 OMPa or less, preferably -0.095 MPa or less, and a stirring speed of 100 rpm to 5 rpm
- the reaction is carried out at a speed of from 00 rpm, preferably from 250 rpm to 400 rpm, from 2 minutes to 30 minutes, preferably from 15 minutes to 25 minutes.
- a two-part outer mold (main mold) made of metal, and a mold composed of a wax molded body and a core integrated with pins are used.
- the core used is a plastic molded body having an external shape corresponding to the internal shape of the body of the hollow ceramic molded body, and a wax molded body having an external shape corresponding to the internal shape of the narrow tube portion of the hollow ceramic molded body. And a metal pin protruding from the wax molded body.
- a gel casting method is adopted.
- the prepared ceramic slurry is poured into the cavity formed by the outer mold and the core of the molding die, and the temperature is 5 ° (: a temperature of up to 50 °, Preferably, it is left for several hours at a temperature of 15 ° C. to 40 ° C.
- the ceramic slurry in the mold is gelled and hardened to form a hollow ceramic molded body.
- the step of releasing the hollow ceramic molded body includes releasing the hollow ceramic molded body in the molding die from the outer mold and the core.
- the hollow ceramic molded body is housed in an oven together with the mold, with the pins constituting the core being pulled out of the wax molded body, and the temperature in the oven is reduced to the temperature of the wax molded body. Set the temperature below the melting temperature, for example, below 60 ° C, and leave it for 10 minutes or more.
- the organic solvent present in the pores of the hollow ceramic molded body thermally expands and is extracted on the outer peripheral side and the inner peripheral side of the hollow ceramic molded body. Then, the extracted organic solvent forms a solvent film between the outer peripheral surface of the hollow ceramic molded body and the inner peripheral surface of the outer mold, and between the inner peripheral surface of the molded body and the outer peripheral surface of the core. I do.
- the temperature in the oven is set to, for example, 65 to 120 ° C., preferably 80 to 100 ° C., and the wax molded body is left for 10 minutes or more to remove the wax molded body from the hollow ceramic molded body. Melts and discharges. Thereafter, the hollow ceramic molded body is taken out of the oven together with the outer mold, and the outer mold is divided to take out the hollow ceramic molded body.
- the core wax molded body present in the hollow ceramic molded body is discharged from the hollow ceramic molded body in a molten state, and the hollow ceramic molded body is released from the core.
- the discharge from the hollow ceramic molded body is performed while the hollow ceramic molded body is in the outer mold.
- the core box molded body thermally expands when it melts, and its thermal expansion force largely acts in the cavity of the hollow ceramic molded body.
- the core wax molded body is melted and discharged while the hollow ceramic molded body is in the outer mold.
- the acting force is received by the outer mold via the hollow ceramic molded body, thereby preventing the hollow ceramic molded body from being damaged by the acting force.
- a solvent film is interposed between the inner peripheral surface of the hollow ceramic molded body and the outer peripheral surface of the box molded body. I have. The solvent film prevents the molten resin from entering the pores of the hollow ceramic molded body when the wax molded body is melted. Thereby, when the hollow ceramic molded body is fired, it is possible to prevent damage such as breakage at the time of firing caused by invasion of the molten wax.
- the hollow ceramic molded body is then released from the outer die.
- a solvent film is interposed between the outer peripheral surface of the hollow ceramic molded body and the inner peripheral surface of the outer mold.
- the hollow ceramic molded body can be released from the outer mold without any resistance due to the action of the solvent film, and the occurrence of damage due to the resistance from the outer mold at the time of release can be prevented. .
- the release means enables the release of the hollow ceramic molded body from the outer mold without any or extremely small shrinkage in the mold and without causing any damage such as slight cracks. Thus, it is possible to prevent the occurrence of damage such as cracks due to shrinkage during molding of the hollow ceramic molded body.
- the calcination and firing process of the hollow ceramic molded body is to convert the hollow ceramic molded body into a sintered body to produce a light emitting container.
- a light-emitting container having high light-transmitting properties and excellent light-transmitting properties can be manufactured.
- the light-emitting container does not have any slight damage such as a crack due to the use of the above-described special releasing means.
- Figure 2 shows the manufacturing process from the preparation of a ceramic slurry, which is a molding slurry, to the production of a solid ceramic molded body, to the production of a container using the solid ceramic molded body as a precursor.
- These manufacturing steps are general manufacturing steps in a manufacturing method according to another embodiment of the present invention, and include a step of preparing a molding slurry, a step of forming a solid ceramic, and a step of forming a solid ceramic molded body. It consists of a mold release step and a calcining and firing step of the solid ceramic molded body.
- the container is manufactured in the order of these steps.
- the method for manufacturing the solid ceramic molded body includes a method for manufacturing a hollow ceramic molded body, Is substantially the same except that the compact to be molded is solid or hollow. That is, in the production of the solid ceramic molded body, a split mold having no core is used as the slurry molding die, and the core wax is used in the mold release of the solid ceramic molded body. There is no need for a means for heating and melting the molded body and discharging it, and no such means has been adopted. However, even in the method for manufacturing a solid ceramic molded body, the heating of the solid ceramic molded body is indispensable when the solid ceramic molded body is released from the mold.
- the solvent existing in the pores of the solid ceramic molded body is thermally expanded and extracted to the outer peripheral side of the molded body.
- the solvent extracted on the outer peripheral side of the solid ceramic molded body forms a solvent film between the outer peripheral surface of the molded body and the inner peripheral surface of each split mold of the molding die. Therefore, the solid ceramic molded body can be released from each split mold without any resistance by the action of the solvent film when the mold is released from each split mold. Can be prevented from being caused by the resistance of the semiconductor device.
- a ceramic slurry (slurry A) for molding a compact having a small body shrinkage of 5% or less in the mold and a body shrinkage rate in the mold were set as the molding slurry.
- a ceramic rally (slurry B) for molding a large molded object of 5% or more an experiment was conducted to produce a hollow ceramic molded body based on each production process in Fig. 1. Tried.
- FIGS. 3 (a) to 3 (c) schematically show the manufacturing process in this experiment
- FIG. 4 (a) shows the process of discharging the core wax molded body in the hollow ceramic molded body in a molten state in this experiment
- Fig. 4 (b) schematically shows the hollow ceramic molded body released from the outer mold in this experiment.
- Table 1 shows the composition and properties of each of the ceramic slurries A and B. Molding slurry
- AKP-20 is manufactured by Sumitomo Chemical Co., Ltd. (trade name)
- Dispersion medium Chemrez 6080 is manufactured by Hodogaya Ashland Co., Ltd. (trade name)
- Reaction catalyst: Kaoriza N025 is manufactured by Kao Corporation (trade name)
- the hollow ceramic molded body manufactured in this experiment has the structure shown in Fig. 4 (b) and is a precursor of the luminous vessel of the high pressure discharge lamp.
- the hollow ceramic molded body 20 is composed of a body 21 corresponding to the body of the light emitting container, and thin tubes 22 and 23 corresponding to the thin tubes of the light emitting container.
- the luminous container is a hollow ceramic
- the compact 20 is calcined at 1200 in the air atmosphere for 3 hours, and then calcined at 1850 ° C. for 3 hours in a hydrogen atmosphere.
- the molding die 10 includes an outer die 11 and a core 12.
- the outer mold 11 is a split type composed of a pair of split molds 1 la and 11 b made of stainless steel, and the inner peripheral shape of the outer mold 11 is the outer peripheral shape of the hollow ceramic molded body 20.
- the core 12 is composed of a wax molded body 12a and a pin 12b, and the outer peripheral surface of the wax molded body 12a has a shape corresponding to the inner peripheral surface of the body 21 of the hollow ceramic molded body 20.
- the outer peripheral surface shape of the pin 12b has a shape corresponding to the inner peripheral surface shape of each of the narrow tube portions 22, 23 of the hollow ceramic molded body 20.
- the melting point of the wax molded body 12a is about 6 O :, and the pin 12b penetrates through the center of the wax molded body 12a, and is formed integrally with the wax molded body 12a at the time of molding. Is what it is.
- the molding of the hollow ceramic molded body 20 is performed with the molding die 10 in a state where the core 12 is set in the outer die 11 as shown in FIG.
- the molding slurry is injected into the cavity 13 through the slurry injection port 11c of the outer mold 11, and the cavity 13 is filled with the molding slurry as shown in FIG. If this state is left at room temperature for several hours, the filled molding slurry gels and hardens.
- the hollow ceramic molded body 20 is molded in the cavity 13.
- the molded hollow ceramic molded body 20 is released from the mold 20.
- the hollow ceramic molded body 20 in the molding die 10 is heated to an appropriate temperature equal to or lower than the temperature at which the wax molded body 12 a of the core 12 is melted, for example, 5 O: Heat to Thereafter, the pins 12b constituting the core 12 are pulled out of the wax molded body 12a and removed from the outer mold 11.
- the wax molded body 12a constituting the core 12 is heated to a temperature of 60 or more, which is the melting temperature.
- the hollow ceramic molded body 20 is released from the core 12 and then the outer die 11 is divided and released from both the divided dies 11a and 11b.
- the organic solvent present in the pores of the hollow ceramic molded body 20 is thermally expanded by the heating of the hollow ceramic molded body 20 and is extracted to the outside of the hollow ceramic molded body. Then, the extracted organic solvent flows between the outer peripheral surface of the hollow ceramic molded body 20 and the inner peripheral surface of the outer mold 11, and between the inner peripheral surface of the hollow ceramic molded body 20 and the outer periphery of the core 12.
- a solvent film which is a film of an organic solvent, is formed between the film and the surface.
- the solvent film located on the inner peripheral surface side of the outer mold 11 contributes to the release of the hollow ceramic molded body 20 from the outer mold 11 and forms the hollow ceramic molded body 20. Release without any resistance.
- the hollow ceramic molded body 20 is free from damage such as breakage when being released from the outer mold 11, and has a small shrinkage in the mold 10, and is difficult to be released. Facilitates demolding of ceramic compacts without causing any damage.
- the solvent film located on the outer peripheral surface side of the core 12 contributes when the box molded body 12a constituting the core 12 is discharged in a molten state.
- the solvent film prevents the molten wax from entering the hollow ceramic molded body 20 when the wax molded body 12a is melted. As a result, when the hollow ceramic molded body 20 is fired, the occurrence of breakage due to the penetrated wax is prevented.
- the wax molded body 12 a constituting the core 12 is discharged in a molten state while the hollow ceramic molded body 20 is in the outer mold 11. .
- the wax molded body 12a thermally expands when heated and melted, and this thermal expansion force acts on the inner peripheral surface side of the hollow ceramic molded body 20.
- the hollow ceramic molded body 20 is in the outer mold 11 and the thermal expansion force is hollow. It is received on the inner peripheral surface side of the outer mold 11 through the ceramic molded body 20.
- a1 indicates that the method of extracting the solvent from the hollow ceramic molded body 20 is used
- bl indicates that the method of extracting the solvent is not used
- the core 12 indicates When the means for discharging the wax molded body 12a in the molten state is in the state where the hollow ceramic molded body 20 is in the outer mold 11, a2, and when the hollow ceramic molded body 20 is removed.
- the case where the removal is performed from the mold 11 is indicated as b2, and the indication is adopted by combining these means.
- the mold releasing means al-a 2 employs a means for extracting the solvent from the hollow ceramic molded body 20 and discharges the wax molded body 12 a in a molten state from the hollow ceramic molded body 2. This means that the operation is performed with 0 being inside the outer mold 1 1.
- the mold releasing means al-b 2 employs a means for extracting a solvent from the hollow ceramic molded body 20, and discharges the wax molded body 12 a in a molten state. It means that the operation is performed with the outer mold taken out from the outer mold.
- the mold releasing means bl-a 2 does not employ a means for extracting the solvent from the hollow ceramic molded body 20, and discharges the wax molded body 12 a in a molten state by the hollow ceramic molded body 2. This means that the operation is performed with 0 being inside the outer mold 1 1.
- the mold release means bl _ b 2 does not employ a means for extracting the solvent from the hollow ceramic molded body 20, and discharges the wax molded body 12 a in a molten state by a hollow ceramic molded body. It means that the operation is performed with 20 being removed from the outer mold 11.
- Table 2 Effect of slurry on damage
- Damage rate indicates the ratio of the molded body and the fired body where damage has occurred per 100 manufactured and fired bodies.
- Damage rate indicates the ratio of the molded body and the fired body where damage has occurred per 100 manufactured and fired bodies.
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Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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CN200380101490.4A CN1705545B (zh) | 2002-10-16 | 2003-10-15 | 制备陶瓷生坯的方法 |
EP03756613A EP1552913A4 (en) | 2002-10-16 | 2003-10-15 | METHOD FOR PRODUCING A CERAMIC FORMK RPTER |
JP2004544955A JP4614767B2 (ja) | 2002-10-16 | 2003-10-15 | セラミック成形体の製造方法 |
US11/085,816 US7517490B2 (en) | 2002-10-16 | 2005-03-21 | Method of manufacturing ceramic green body |
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JP2002-302013 | 2002-10-16 | ||
JP2002302013 | 2002-10-16 |
Related Child Applications (1)
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US11/085,816 Continuation US7517490B2 (en) | 2002-10-16 | 2005-03-21 | Method of manufacturing ceramic green body |
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WO2004035281A1 true WO2004035281A1 (ja) | 2004-04-29 |
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PCT/JP2003/013163 WO2004035281A1 (ja) | 2002-10-16 | 2003-10-15 | セラミック成形体の製造方法 |
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EP (1) | EP1552913A4 (ja) |
JP (1) | JP4614767B2 (ja) |
CN (1) | CN1705545B (ja) |
WO (1) | WO2004035281A1 (ja) |
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JP2008518403A (ja) * | 2004-10-26 | 2008-05-29 | ゼネラル・エレクトリック・カンパニイ | 一体的に形成された成型部分およびその作成方法 |
WO2009110579A1 (ja) * | 2008-03-06 | 2009-09-11 | 日本碍子株式会社 | セラミックグリーンシート、及びセラミックグリーンシート積層体、並びに、セラミックグリーンシートの製造方法、及びセラミックグリーンシート積層体の製造方法 |
WO2010079729A1 (ja) | 2009-01-06 | 2010-07-15 | 日本碍子株式会社 | 成形型、及び、その成形型を用いた成形体の製造方法 |
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JP4614767B2 (ja) | 2011-01-19 |
CN1705545A (zh) | 2005-12-07 |
JPWO2004035281A1 (ja) | 2006-02-09 |
CN1705545B (zh) | 2010-05-05 |
EP1552913A1 (en) | 2005-07-13 |
EP1552913A4 (en) | 2008-05-07 |
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