WO2004067475A1 - グリーンシート用塗料とその製造方法、グリーンシートとその製造方法、及び電子部品の製造方法 - Google Patents
グリーンシート用塗料とその製造方法、グリーンシートとその製造方法、及び電子部品の製造方法 Download PDFInfo
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- WO2004067475A1 WO2004067475A1 PCT/JP2004/000755 JP2004000755W WO2004067475A1 WO 2004067475 A1 WO2004067475 A1 WO 2004067475A1 JP 2004000755 W JP2004000755 W JP 2004000755W WO 2004067475 A1 WO2004067475 A1 WO 2004067475A1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/02—Homopolymers or copolymers of unsaturated alcohols
- C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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Definitions
- Green sheet paint and its manufacturing method Green sheet and its manufacturing method
- the present invention relates to a paint for a green sheet, a green sheet, a method for producing a paint for a green sheet, a method for producing a green sheet, and a method for producing an electronic part, and more particularly, to an extremely thin sheet.
- the present invention relates to a paint and a green sheet coating method capable of manufacturing a Darin sheet excellent in handling and adhesion, suitable for thinning and multilayering of electronic components.
- the thickness of the dielectric green sheet constituting the dielectric layer has been reduced to several ⁇ or less.
- ceramic powder In order to manufacture ceramic green sheets, ceramic powder, binders (acrylic resin, butyral resin, etc.), plasticizers (phthalates, glycols, adipic acid, phosphates) and organic solvents are usually used first.
- binders acrylic resin, butyral resin, etc.
- plasticizers phthalates, glycols, adipic acid, phosphates
- organic solvents Toluene, ME Prepare a ceramic paint consisting of K, acetone, etc.).
- the ceramic paint is applied on a carrier sheet (support made of ⁇ ⁇ ⁇ and ⁇ ⁇ ) using a doctor blade method or the like, and heated and dried to manufacture.
- a method for manufacturing a multilayer ceramic capacitor using the above-described ceramic green sheets will be specifically described.
- a conductive paste for an internal electrode including a metal powder and a binder is printed in a predetermined pattern on a ceramic green sheet and dried to form an internal electrode pattern. Thereafter, the green sheet is peeled off from the carrier sheet, and this is laminated to a desired number of layers.
- two types of methods have been devised: a method of peeling the green sheet from the carrier sheet before lamination and a method of peeling the carrier sheet after lamination and pressure bonding, but there is no significant difference.
- the laminate is cut into chips to form green chips. After firing these green chips, external electrodes are formed to manufacture electronic components such as multilayer ceramic capacitors.
- the interlayer thickness of the sheet on which the internal electrodes are formed is about 3 ⁇ ! Based on the desired capacitance required for the capacitor. It is in the range of about 100 ⁇ . Further, in the multilayer ceramic capacitor, a portion where an internal electrode is not formed is formed on an outer portion of the capacitor chip in the stacking direction.
- Patent Document 1 see Japanese Patent Application Laid-Open No. H10-667567). The reasons for this are to ensure sufficient adhesion of the ceramic green sheets during lamination, to reduce the surface roughness of the green sheets, To secure the flexibility of the sheet and to lower the viscosity of the slurry.
- the plasticizer phthalic acid, adipic acid, sebacic acid, and phosphoric esters can be generally used, but are selected from the viewpoints of boiling point and harmfulness for the purpose of imparting plasticity. Was.
- the properties required for the physical properties of such extremely thin green sheets include sheet strength, flexibility, smoothness, adhesion during lamination, and handling (charging). Is required.
- Patent Document 2 Japanese Patent Application Laid-Open No. 6-206756
- a polybutylene having a degree of polymerization of 100 or more is used in order to eliminate short-circuit defects.
- a technique using a petital resin as a binder is known.
- Patent Document 2 does not particularly aim at reducing the thickness of the organic solvent-based green sheet, nor does it limit the range of the degree of polymerization of the polybierptylal resin to a specific range. Further, no attention is paid to the butyralization degree and the residual acetyl group content of the resin.
- An object of the present invention is to remove even a very thin green sheet from a support.
- Another object of the present invention is to provide a method of manufacturing an electronic component suitable for making the electronic component thinner or more multilayered.
- the present inventor has found that the use of a polyvinyl acetal resin having a specific range of polymerization degree, a specific range of degree of butyralization, and a residual acetyl group amount of a predetermined value or less as a binder makes it extremely possible. It has been found that, even with a thin resin green sheet, it is possible to produce a green sheet having strength enough to withstand peeling from a support and having good adhesive and handling properties. We have completed this invention. -[0 0 1 5]
- the green sheet paint according to the first aspect of the present invention is a green sheet paint comprising a ceramic powder, a pinda resin, a plasticizer, and a solvent,
- the binder resin contains a polyvinyl butyral resin, the degree of polymerization of the polybutyral resin is 10000 or more and 1700 or less, and the nominal value of the degree of butyralization of the resin is 65% or more and 78% or more. It is small and the residual acetyl group content is less than 6%.
- the solvent is not particularly limited, but an organic solvent is preferably used. Note that the nominal value of the degree of Petitlar varies in the range of ⁇ 3%. That is, a nominal value of the degree of butyralization of 65% means 65 ⁇ 3%. In the following description, the term “degree of butyralization” simply means “the nominal value of the degree of butyralization”.
- the degree of polymerization of the polybutyral resin if the degree of polymerization of the polybutyral resin is too small, sufficient mechanical strength tends to be hardly obtained, for example, when the thickness is reduced to, for example, preferably about 3 m or less.
- the degree of polymerization if the degree of polymerization is too large, the surface roughness when formed into a sheet tends to deteriorate.
- polybutyral resin blocks If the chillalization degree is too low, the solubility in the paint tends to deteriorate, and if it is too high, the sheet surface roughness tends to deteriorate. Further, if the residual acetyl group content is too large, the sheet surface roughness tends to deteriorate.
- a very thin dary sheet has strength enough to withstand peeling from a support, and has good adhesion and handling properties.
- a green sheet having the same can be manufactured.
- a green sheet paint comprising a ceramic powder, a pinda resin, a plasticizer, and an organic solvent
- Water is contained in an amount of 1 part by mass or more and 6 parts by mass or less based on 100 parts by mass of the ceramic powder.
- the water content is too small, the change in paint properties over time due to moisture absorption becomes large, which is not preferable, and the viscosity of the paint tends to increase, and the filtration property of the paint tends to deteriorate.
- the water content is too high, the paint tends to separate or settle, the dispersibility becomes poor, and the surface roughness of the sheet tends to deteriorate.
- a green sheet paint comprising a ceramic powder, a binder resin, a plasticizer, a solvent, and a dispersant
- the dispersant comprises a polyethylene glycol-based nonionic dispersant, 'The lipophilic balance (HLB (Hydrophilic Lipophilic Balance)) value is 5-6,
- the dispersant is added in an amount of 0.5 to 1.5 parts by mass based on 100 parts by mass of the ceramic powder.
- the dispersant is a dispersant other than a polyethylene dalicol-based nonionic dispersant
- the paint viscosity increases, the sheet density decreases, the sheet surface roughness increases, and the sheet elongation decreases. Or tend to.
- the HLB of the dispersant is outside the above range, the sheet density tends to decrease and the sheet surface roughness tends to increase.
- even a very thin Darine sheet has strength enough to withstand peeling from a support, and has good adhesion and handling properties. Green sheets can be manufactured.
- the amount of the dispersant added is too small, the viscosity of the coating material increases, the sheet density decreases, and the sheet surface roughness tends to increase.
- the amount is too large, the tensile strength of the sheet tends to decrease and the adhesiveness tends to decrease.
- a paint for a green sheet comprising a ceramic powder, a pinda resin, a plasticizer, a solvent, and a charge aid,
- the antistatic agent includes an imidazoline-based antistatic agent, and the charging aid is included in an amount of 0.1 to 0.75 parts by mass with respect to 100 parts by mass of the ceramic powder.
- the antistatic agent when the antistatic agent is other than an imidazoline-based antistatic agent, the effect of removing static electricity is small, and the sheet strength, sheet elongation or adhesiveness tends to deteriorate.
- the paint for green sea 1 and the fourth aspect of the present invention even if the green sheet is extremely thin, the green sheet has strength enough to withstand peeling from the support. It is possible to produce a green sheet which suppresses generated static electricity and has good adhesive and handling properties.
- the amount of the antistatic agent is too small, the amount of the antistatic agent is reduced If the effect is small and too large, the surface roughness of the sheet tends to deteriorate and the sheet strength tends to deteriorate.
- a green sheet paint comprising a ceramic powder, a binder resin, a solvent, and if necessary, a plasticizer and a dispersant,
- the solvent contains an alcohol solvent and an aromatic solvent, and the total weight of the alcohol solvent and the aromatic solvent is 100 parts by mass, and the aromatic solvent is 10 parts by mass or more and 20 parts by mass. Parts or less are included. If the content of the aromatic solvent is too small, the surface roughness of the sheet tends to increase, and if it is too high, the paint filtration characteristics deteriorate and the sheet surface roughness also increases.
- the binder resin is contained in an amount of 5 parts by mass or more and 6.5 parts by mass or less based on 100 parts by mass of the ceramic powder. If the content of the pinda resin is too small, the sheet strength tends to decrease and the stacking property (adhesion at the time of lamination) tends to deteriorate. On the other hand, if the binder resin content is too large, segregation of the binder resin tends to occur and dispersibility tends to deteriorate, and the sheet surface roughness tends to deteriorate.
- dioctyl phthalate is contained as the plasticizer in an amount of from 40 to 70 parts by mass based on 100 parts by mass of the binder resin.
- dioctyl phthalate is preferred in terms of both sheet strength and sheet elongation, and is particularly preferred because of its low peel strength from the support and easy peeling. If the content of the plasticizer is too small, the sheet elongation tends to be small and the flexibility tends to be small. On the other hand, if the content is too large, the plasticizer will be blown out of the sheet, and the plasticizer tends to be deflected to the sheet, and the dispersibility of the sheet tends to decrease.
- the volume ratio occupied by the ceramic powder is 64.3% or more and 72% or less. . If this volume ratio is too small, the binder will be prayed. And the dispersibility tends to deteriorate, and the surface roughness tends to deteriorate. On the other hand, if the volume ratio is too large, the sheet strength tends to decrease and the stacking property tends to deteriorate.
- At least one of a hydrocarbon solvent, industrial gasoline, kerosene, and solvent naphtha is added to the ceramic powder (100 parts by mass) in an amount of 3 parts by mass to 15 parts by mass. ing.
- a hydrocarbon solvent industrial gasoline, kerosene, and solvent naphtha
- the sheet strength and the sheet surface roughness can be improved. If the amount of these additives is too small, the effect of the addition is small, and if the amount is too large, the sheet strength and the sheet surface roughness tend to deteriorate.
- the above-mentioned pinda resin is previously dissolved and filtered in at least one or more alcoholic solvents of methanol, ethanol, propanol and butanol to form a solution. It is characterized by adding components.
- a high polymerization degree pinda resin is hardly soluble in a solvent, and the dispersibility of a coating material tends to be deteriorated by an ordinary method.
- the dispersibility of the paint is improved by dissolving the high polymerization degree pinda resin in the above-mentioned good solvent and then adding the ceramic powder and other components to the solution. And the generation of undissolved resin can be suppressed.
- the solid content concentration cannot be increased, and the change over time in the rubbing force-viscosity tends to increase.
- the method for producing a green sheet according to the present invention comprises:
- the green sheet according to the present invention is manufactured by using the green sheet paint.
- FIG. 1 is a schematic cross-sectional view of a multilayer ceramic capacitor according to an embodiment of the present invention
- FIGS. 2A to 2C are main-portion cross-sectional views illustrating a method of transferring an electrode layer
- FIG. 3A to FIG. 3C are cross-sectional views of relevant parts showing a process subsequent to FIG.
- 4A to 4C are cross-sectional views of a main part showing a method of laminating a green sheet to which an electrode layer is adhered.
- 5A to 5C are cross-sectional views of a main part showing a method for laminating a green sheet to which an electrode layer is adhered, showing a process subsequent to FIG.
- 6A to 6C are cross-sectional views of a main part showing a step subsequent to that of FIG. 5,
- FIG. 7 is an essential part cross-sectional view showing a step subsequent to FIG. 6,
- FIG. 8 is a fragmentary cross-sectional view showing a step that follows the step shown in FIG.
- the multilayer ceramic capacitor 2 has a capacitor body 4, a first terminal electrode 6, and a second terminal electrode 8.
- the capacitor body 4 has a dielectric layer 10 and an internal electrode layer 12, and the internal electrode layers 12 are alternately stacked between the dielectric layers 10.
- One of the alternately laminated internal electrode layers 12 is electrically connected to the inside of the first terminal electrode 6 formed outside one end of the capacitor body 4.
- the other internal electrode layers 12 alternately stacked are electrically connected to the inside of the second terminal electrode 8 formed outside the other end of the capacitor body 4.
- the internal electrode layer 12 is formed by transferring the electrode layer 12a to the ceramic green sheet 10a as shown in FIGS. 2 to 6, as will be described later in detail. .
- the material of the dielectric layer 10 is not particularly limited, and is made of a dielectric material such as calcium titanate, strontium titanate and / or barium titanate.
- the thickness of each dielectric layer 10 is not particularly limited, but is generally several im to several hundred ⁇ . In particular, in the present embodiment, the thickness is reduced to preferably 5 m or less, more preferably 3 ⁇ m or less.
- the material of the terminal electrodes 6 and 8 is also not particularly limited. Usually, copper, a copper alloy, a nickel-nickel alloy, or the like is used, but silver or an alloy of silver and palladium can also be used.
- the thickness of the terminal electrodes 6 and 8 is not particularly limited, but is usually about 10 to 50 ⁇ .
- the shape and size of the multilayer ceramic capacitor 2 can be appropriately determined according to the purpose and application.
- the dielectric paint is composed of an organic solvent-based paint obtained by kneading a dielectric material (ceramic powder) and an organic vehicle.
- the dielectric material various compounds that can be used as composite oxides and oxides, for example, carbonates, nitrates, hydroxides, organometallic compounds, and the like can be appropriately selected and used as a mixture.
- the dielectric material usually has an average particle size of 0 or less, preferably 0.
- the organic vehicle is obtained by dissolving a pinda resin in an organic solvent.
- a polybutyral resin is used as the binder resin used for the organic vehicle.
- the polymerization degree of the polybutyral resin is from 1,000 to 1,700, and preferably from 1,400 to 1,700.
- the degree of butyralization of the resin is 65% or more and less than 78%, preferably 65% or more and 70% or less, and the residual acetyl group content is less than 6%, preferably 3% or less.
- the degree of polymerization of the polybutyral resin can be measured, for example, by the degree of polymerization of the polyvinyl acetal resin as a raw material.
- the degree of Petitiral It can be measured according to SK6728.
- the amount of the residual acetyl group can be measured according to JISK6728.
- the degree of polymerization of the polybutyral resin is too small, sufficient mechanical strength tends to be hardly obtained, for example, when the thickness is reduced to 5 / im or less, preferably about 3 ⁇ or less.
- the degree of polymerization is too large, the surface roughness when formed into a sheet tends to deteriorate.
- the degree of polybutyral of the polybutylal resin is too low, the solubility in the coating tends to deteriorate, and if it is too high, the sheet surface roughness tends to deteriorate. Further, if the residual acetyl group content is too large, the sheet surface roughness tends to deteriorate.
- the organic solvent used for the organic vehicle is not particularly limited, and for example, organic solvents such as terbineol, alcohol, butyl carbitol, acetone, and toluene are used.
- the organic solvent preferably includes an alcohol solvent and an aromatic solvent, and the total mass of the alcohol solvent and the aromatic solvent is 100 parts by mass, and the aromatic solvent is But not less than 10 parts by mass and not more than 20 parts by mass. If the content of the aromatic solvent is too small, the surface roughness of the sheet tends to increase, and if it is too large, the paint filtration characteristics deteriorate and the sheet surface roughness also increases and deteriorates.
- alcohol solvents examples include methanol, ethanol, propanol, butanol and the like.
- aromatic solvent examples include toluene, xylene, and benzyl acetate.
- the binder resin is previously dissolved and filtered in at least one or more of alcoholic solvents of methanol, ethanol, propanol, and butanol to form a solution. It is preferred to add components.
- a binder resin having a high polymerization degree is hardly soluble in a solvent, and the dispersibility of a coating material tends to be deteriorated by an ordinary method.
- a high polymerization degree of the pinda resin is dissolved in the above-mentioned good solvent, and then the ceramic powder and other components are added to the solution. Therefore, the dispersibility of the paint can be improved, and the generation of undissolved resin can be suppressed.
- the solid content concentration cannot be increased, and the change over time in the rubbing force-viscosity tends to increase.
- the dielectric coating may optionally contain additives selected from various dispersants, plasticizers, antistatic agents, dielectrics, glass frit, insulators, and the like.
- the dispersant is not particularly limited, but a polyethylene glycol-based nonionic dispersant is preferably used, and its hydrophilicity / lipophilic balance is preferably used.
- the dispersant is preferably added in an amount of 0.5 to 1.5 parts by mass, more preferably 0.5 to 1.0 parts by mass, based on 100 parts by mass of the ceramic powder. .
- the amount of the dispersant is too small, the sheet surface roughness tends to increase, and if too much, the sheet tensile strength and the stacking property tend to decrease.
- dioctyl phthalate is preferably used, and it is preferably 40 to 70 parts by mass, more preferably 40 to 6 parts by mass, based on 100 parts by mass of the binder resin. It is contained at 0 parts by mass.
- dioctyl phthalate is preferred in terms of both sheet strength and sheet elongation, and is particularly preferred because of its low peel strength from the support and easy peeling. If the content of the plasticizer is too small, the sheet elongation tends to be small and the flexibility tends to be small. On the other hand, if the content is too large, the plasticizer bleeds out of the sheet, so that the plasticizer tends to be deflected to the sheet, and the dispersibility of the sheet tends to decrease.
- the dielectric paint contains water in an amount of 1 to 6 parts by mass, preferably 1 to 3 parts by mass, based on 100 parts by mass of the dielectric powder.
- Water If the content is too small, the change over time in the paint properties due to moisture absorption becomes large, which is not preferable, and the viscosity of the paint tends to increase, and the filtration property of the paint tends to deteriorate. On the other hand, if the water content is too large, the paint tends to separate or settle, the dispersibility becomes poor, and the surface roughness of the sheet tends to deteriorate.
- At least one of a hydrocarbon solvent, industrial gasoline, kerosene, and solvent naphtha is preferably used in an amount of 3 parts by mass or more based on 100 parts by mass of the dielectric powder. It is added in an amount of 5 parts by mass or less, more preferably 5 to 10 parts by mass.
- the binder resin is preferably contained in an amount of 5 parts by mass or more and 6.5 parts by mass or less based on 100 parts by mass of the dielectric powder. If the content of the pinda resin is too small, the sheet strength tends to decrease and the stacking property (adhesion at the time of lamination) tends to deteriorate. On the other hand, if the content of the pinda resin is too large, the dispersibility of the pinda resin tends to deteriorate, and the sheet surface roughness tends to deteriorate.
- the volume ratio occupied by the dielectric powder is preferably 62.42% or more and 72.6%.
- the content is 9% or less, more preferably 63.93% or more and 72.69% or less. If the volume ratio is too small, pinda's bias tends to occur, dispersibility tends to be poor, and surface roughness tends to deteriorate. On the other hand, if the volume ratio is too large, the sheet strength tends to decrease and the stacking property tends to deteriorate.
- the dielectric paint preferably contains an antistatic agent
- the charge assistant is preferably an imidazoline-based antistatic agent.
- the antistatic agent is other than an imidazoline-based antistatic agent, the effect of removing static electricity is small, and the sheet strength, sheet elongation, or adhesiveness tends to deteriorate.
- the charging aid is contained in an amount of 0.1 to 0.75 parts by mass, more preferably 0.25 to 0.5 parts by mass, per 100 parts by mass of the ceramic powder. If the added amount of the antistatic agent is too small, the effect of removing static electricity is reduced, and if it is too large, the surface roughness of the sheet and the sheet strength tend to deteriorate. If the effect of removing static electricity is small, static electricity is likely to be generated when the carrier sheet 30 as a support is peeled from the ceramic green sheet 10a, and disadvantages such as wrinkling of the green sheet are likely to occur.
- a carrier sheet 30 as a second support sheet by a doctor blade method or the like, preferably 0.5 to 30 ⁇ , more preferably 0.5 to 0.5 ⁇ .
- a green sheet 10a is formed with a thickness of about 10 ⁇ .
- the green sheet 10a is dried after being formed on the carrier sheet 30.
- the drying temperature of the green sheet 10a is preferably 50 to 100 ° C, and the drying time is preferably 1 to 20 minutes.
- the thickness of the green sheet 10a after drying shrinks to 5 to 25% of the thickness before drying.
- the thickness of the green sheet after drying is preferably 3 Attn or less.
- a carrier sheet 20 as a first support sheet is prepared, and a release layer 22 is formed thereon. Further, an electrode layer 12a having a predetermined pattern is formed thereon, and before and after that, on the surface of the release layer 22 where the electrode layer 12a is not formed, the thickness is substantially the same as that of the electrode layer 12a. Only the blank pattern layer 24 is formed.
- the carriers 20 and 30 for example, PET films and the like are used, and those coated with silicon or the like to improve the releasability are preferable.
- the thickness of the carrier sheets 20 and 30 is not particularly limited, but is preferably 5 to 100 ⁇ . The thickness of these carrier sheets 20 and 30 may be the same or different.
- the release layer 22 preferably contains the same dielectric particles as the dielectric constituting the green sheet 10a shown in FIG. 3A.
- the release layer 22 contains a binder, a plasticizer, and a release agent in addition to the dielectric particles.
- the particle size of the dielectric particles may be the same as the particle size of the dielectric particles contained in the green sheet, but is preferably smaller.
- the thickness t2 of the release layer 22 is preferably not more than the thickness of the electrode layer 12a, preferably not more than 60%, more preferably not more than 30%. I do.
- the method of applying the release layer 22 is not particularly limited, but it is necessary to use a wire bar coater or a die coater, for example, since it is necessary to form the release layer 22 extremely thin.
- the thickness of the release layer can be adjusted by selecting a wire and a bar coater having different diameters. That is, in order to reduce the coating thickness of the release layer, one having a small diameter of the wire may be selected, and in order to form a thick layer, one having a large diameter of the wire may be selected.
- the release layer 22 is dried after the application.
- the drying temperature is preferably from 50 to 100 ° C., and the drying time is preferably from 1 to 10 minutes.
- the binder for the release layer 22 is made of, for example, an organic material or an emulsion made of an acryl resin, a polyvinyl butyral / polyvinylacetanol, a polyvinylinole cornole, a polyolefin, a polyurethane, a polystyrene, or a copolymer thereof.
- the binder contained in the release layer 22 may be the same as or different from the binder contained in the green sheet 10a, but is preferably the same.
- plasticizer for the release layer 22 examples include, but are not particularly limited to, phthalic acid esters, dioctyl phthalate, adipic acid, phosphoric acid esters, and glycols.
- the plasticizer contained in the release layer 22 may be the same as or different from the plasticizer contained in the green sheet 10a.
- the release agent for the release layer 22 is not particularly limited, and examples include paraffin, wax, and silicone oil. Release agent contained in the release layer 2 2 may be the same or different as the release agent contained in the green sheet Ichito 1 0 a.
- the binder is contained in the release layer 22 in an amount of preferably 2.5 to 200 parts by mass, more preferably 5 to 30 parts by mass, and particularly preferably about 8 to 30 parts by mass with respect to 100 parts by mass of the dielectric particles. Included in.
- the plasticizer is preferably contained in the release layer 22 in an amount of 0 to 200 parts by mass, preferably 20 to 200 parts by mass, more preferably 50 to 100 parts by mass, based on 100 parts by mass of the binder. .
- the release agent is preferably contained in the release layer 22 in an amount of 0 to 100 parts by mass, preferably 2 to 50 parts by mass, and more preferably 5 to 20 parts by mass with respect to 100 parts by mass of the binder.
- the electrode layer 12 a that will constitute the internal electrode layer 12 after firing is formed on the surface of the release layer 22. Formed in a pattern.
- the thickness of the electrode layer 12a is preferably about 0.1 to 2 ⁇ m, and more preferably about 0.1 to 1.1 ⁇ m.
- the electrode layer 12a may be composed of a single layer, or may be composed of two or more layers having different compositions.
- the electrode layer 12a can be formed on the surface of the release layer 22 by a thick film forming method such as a printing method using an electrode paint, or a thin film method such as evaporation or sputtering.
- a thick film forming method such as a printing method using an electrode paint, or a thin film method such as evaporation or sputtering.
- a screen printing method or a gravure printing method which is a kind of a thick film method
- a row 5 is as follows. [0 0 6 8]
- the electrode paint is prepared by kneading an organic vehicle with a conductive material made of various conductive metals or alloys, or various oxides, organometallic compounds, or resinates that become the above-mentioned conductive material after firing.
- the conductor material used in producing the electrode paint Ni, Ni alloy, or a mixture thereof is used.
- the shape of such a conductive material is not particularly limited, such as a sphere or a scale, and a mixture of these shapes may be used.
- the average particle diameter of the conductor material is usually about 0.1 to 2 zm, preferably about 0.2 to 1 / im.
- the organic vehicle contains a pinda and a solvent.
- the pinda include ethyl cellulose, acrylic resin, polybutyral, polyvinyl alcohol, polybutyl alcohol, polyolefin, polyurethane, polystyrene, and copolymers thereof, and in particular, polybutyl butyral and the like. Is preferred.
- the binder is preferably contained in the electrode paint in an amount of 8 to 20 parts by mass with respect to 100 parts by mass of the conductive material (metal powder).
- the solvent any known solvents such as terbineol, butyrcarbitol, and kerosene can be used.
- the solvent content is preferably about 20 to 55% by mass with respect to the entire coating material.
- the electrode paint contains a plasticizer.
- the plasticizer include phthalic acid esters such as benzyl butyl phthalate (BBP), adipic acid, phosphoric acid esters, and glycols.
- the plasticizer is preferably used in an amount of 100 to 300 parts by mass, more preferably 10 to 200 parts by mass, based on 100 parts by mass of the binder. If the amount of the plasticizer or the pressure-sensitive adhesive is too large, the strength of the electrode layer 12a tends to be significantly reduced. Also, in order to improve the transferability of the electrode layer 12a, add a plasticizer or adhesive in the electrode paint. It is preferable to improve the adhesion and / or tackiness of the electrode paint by adding it.
- the electrode layer 1 2 is formed on the surface of the release layer 22 where the electrode layer 12 a is not formed.
- a blank pattern layer 24 having substantially the same thickness as a is formed.
- the blank pattern layer 24 is made of the same material as the green sheet 10a shown in FIG. 3A, and is formed by the same method.
- the electrode layer 12a and the blank pattern layer 12a are dried if necessary.
- the drying temperature is not particularly limited, but is preferably 70 to 120 ° C., and the drying time is preferably 5 to 15 minutes.
- an adhesive layer 28 is formed on the surface of a carrier sheet 26 as a third support sheet.
- the carrier sheet 26 is composed of a sheet similar to the carrier sheet 20 and 30.
- the composition of the adhesive layer 28 is the same as that of the release layer 22 except that it does not contain a release agent. That is, the adhesive layer 28 includes a binder, a plasticizer, and a release agent.
- the adhesive layer 28 may include the same dielectric particles as the dielectric constituting the green sheet 10a. If an adhesive layer having a thickness smaller than the particle diameter of the dielectric particles is formed, the dielectric layer It is better not to include body particles. When the adhesive layer 28 contains dielectric particles, the particle size of the dielectric particles is preferably smaller than the particle size of the dielectric particles contained in the green sheet.
- the plasticizer is contained in the adhesive layer 28 in an amount of 0 to 200 parts by mass, preferably 20 to 200 parts by mass, more preferably 50 to 100 parts by mass, based on 100 parts by mass of the binder. It is preferred that it is included in a part.
- the adhesive layer 28 further includes an antistatic agent.
- the antistatic agent includes one of imidazoline-based surfactants. Material) is preferably not more than the weight-based addition amount. That is, the antistatic agent is contained in the adhesive layer 28 in an amount of 0 to 200 parts by mass, preferably 20 to 200 parts by mass, more preferably 50 to 200 parts by mass, based on 100 parts by mass of the binder. It is preferably contained in 100 parts by mass.
- the thickness of the adhesive layer 28 is preferably about 0.02 to 0.3 ⁇ , and is preferably smaller than the average particle diameter of the dielectric particles contained in the green sheet. Further, it is preferable that the thickness of the adhesive layer 28 is not more than 10 times the thickness of the green sheet 10a.
- the thickness of the adhesive layer 28 is too thin, the adhesive strength is reduced, and if it is too thick, a gap is easily formed inside the element body after sintering depending on the thickness of the adhesive layer. The capacity tends to decrease significantly.
- the adhesive layer 28 is formed on the surface of the carrier sheet 26 as the third support sheet by, for example, a bar coater method, a die coater method, a reverse coater method, a dip coater method, a kiss coater method, and the like. And dried.
- the drying temperature is not particularly limited, but is preferably room temperature to 80 ° C., and the drying time is preferably 1 to 5 minutes.
- a transfer method is employed in the present embodiment. That is, as shown in FIG. 2B, the adhesive layer 28 of the carrier sheet 26 is pressed against the surfaces of the electrode layer 12a and the margin pattern layer 24, heated and pressed, and then the carrier sheet 26 is peeled off. Go. As a result, as shown in FIG. 2C, the adhesive layer 28 is transferred to the surfaces of the electrode layer 12a and the blank pattern layer 24. The transfer of the adhesive layer 28 may be performed on the surface of the green sheet 10a shown in FIG. 3A.
- the heating temperature during the transfer is preferably 40 to 100 ° C., and the pressure is 0.2. ⁇ 15 MPa is preferred.
- the pressurization may be performed by a press or a calender roll, but is preferably performed by a pair of rolls.
- the electrode layer 12a is adhered to the surface of the green sheet 10a formed on the surface of the carrier sheet 30 shown in FIG. 3A.
- the electrode layer 12 a and the blank pattern layer 24 of the carrier sheet 20 are attached to the carrier sheet 20 a via the adhesive layer 28 on the surface of the carrier sheet 10 a. And heat and press.
- the electrode layer 12a and the blank pattern layer 24 are transferred to the surface of the green sheet 10a.
- the carrier sheet 30 on the Darling sheet side is peeled off, when viewed from the green sheet 10a side, the green sheet 10a is bonded to the electrode layer 12a and the blank pattern layer 24 by the adhesive layer 2. Transcribed through 8.
- the heating and pressurizing during the transfer may be pressurizing and heating by a press or pressurizing and heating by a calendar roll, but are preferably performed by a pair of rolls.
- the heating temperature and the pressing force are the same as when transferring the adhesive layer 28.
- a single layer of the electrode layer 12a having a predetermined pattern is formed on the single green sheet 10a.
- the steps shown in FIGS. 4A to 6C may be repeated.
- members common to those shown in FIGS. 3A to 4C are denoted by the same reference numerals, and description thereof is partially omitted.
- the adhesive layer 28 is transferred to the surface (rear surface) on the side opposite to the electrode layer in the green sheet 10a. Thereafter, as shown in FIGS. 5A to 5C, the electrode layer 12a and the blank pattern layer 24 are transferred to the back surface of the green sheet 10a via the adhesive layer 28.
- the electrode layers 12 a and ⁇ ⁇ ⁇ ⁇ Transfer the green sheet 10a to the surface of the margin pattern layer 24. Thereafter, by repeating these transfers, a laminated block in which a large number of electrode layers 12a and green sheets 10a are alternately laminated as shown in FIG. 7 is obtained.
- the following steps may be performed without employing the steps shown in FIGS. 5C to 6C. That is, instead of peeling the lower carrier sheet 20 from the step shown in FIG. 5B, the upper carrier sheet is peeled off, and the laminate unit U1 shown in FIG. 4C is laminated thereon. good. Thereafter, the upper carrier sheet 20 is again peeled off, the laminate unit U1 shown in FIG. 4C is laminated thereon, and the operation of peeling the upper carrier sheet 20 again is repeated. As shown in FIG. 7, a laminated block in which a large number of electrode layers 12a and green sheets 10a are alternately laminated is obtained. The method of laminating the laminate unit U1 shown in FIG. 4C is superior in lamination work efficiency.
- the firing step in the next step is performed using the stacked block alone. Further, if necessary, such a plurality of laminated blocks may be laminated via an adhesive layer 28 formed by a transfer method in the same manner as described above to form a more multilayer laminated body.
- a green sheet 40 for an outer layer (a thick laminate obtained by laminating a plurality of green sheets on which no electrode layer is formed) is laminated. Then, the entire laminate is supported by the suction holding table 50. Thereafter, the upper carrier sheet 20 is peeled off, and a green sheet 40 for the outer layer is similarly formed on the top of the laminate, followed by final pressing.
- the pressure at the time of final pressurization is preferably 10 to 20 O MPa.
- the heating temperature is preferably from 40 to 100 ° C.
- the laminated body is cut into a predetermined size to form a daline chip.
- the green chip is subjected to a binder removal treatment and a baking treatment, and then a heat treatment is performed to reoxidize the dielectric layer.
- the binder removal treatment may be performed under ordinary conditions. However, when a base metal such as Ni or Ni alloy is used as the conductor material of the internal electrode layer, it is particularly preferable to perform the treatment under the following conditions.
- Heating rate 5 ⁇ 300 ° CZ time, especially 10 ⁇ 50 ° C / hour,
- Holding temperature 200 ⁇ 400 ° C, especially 250 ⁇ 350 ° C,
- Holding time 0.5 to 20 hours, especially 1 to: L 0 hours,
- Atmosphere wet mixed gas of N 2 and H 2.
- the firing conditions are preferably as follows.
- Heating rate 50 ⁇ 500 ° CZ time, especially 200 ⁇ 300 ° C / hour,
- Holding temperature 1 100-1300 ° C, especially 1 150-1250 ° C
- Holding time 0.5-8 hours, especially 1-3 hours
- Cooling rate 50 ⁇ 500 ° C / hour, especially 200 ⁇ 300 ° CZ time
- Atmosphere gas A humidified gas mixture of N 2 and H 2 .
- the oxygen partial pressure in an air atmosphere at firing is less 10-2 P a, it is preferably carried out in particular 10- 2-10 one 8 P a. If it exceeds the above range, the internal electrode layer tends to be oxidized. If the oxygen partial pressure is too low, the electrode material of the internal electrode layer tends to be abnormally sintered and cut off.
- the heat treatment after the firing is preferably performed at a holding temperature or a maximum temperature of preferably 1000 ° C. or higher, more preferably 1000 to 1100 ° C. If the holding temperature or the maximum temperature during the heat treatment is less than the above range, the insulation resistance life tends to be short due to insufficient oxidation of the dielectric material, and if the holding temperature or the maximum temperature exceeds the above range, Ni of the internal electrode is oxidized and the capacity is increased. Not only does it decrease, it also reacts with the dielectric substrate, and its life tends to be shortened.
- Oxygen partial pressure at the thermal treatment is higher oxygen partial pressure than the reduction Kiri ⁇ gas during firing, preferably 10- 3 P a ⁇ 1 P a, more preferably 10- 2 P a ⁇ 1 P a is there. Below this range, re-oxidation of the dielectric layer 2 is difficult, and beyond this range, the internal electrode layer 3 tends to be oxidized. And other The heat treatment conditions are preferably the following conditions.
- Retention time 0-6 hours, especially 2-5 hours
- Cooling rate 500 ⁇ 500 ° C / hour, especially 100 ⁇ 300 ° C / hour,
- Atmosphere gas Humidified N 2 gas, etc.
- a wetter may be used.
- the water temperature is preferably about 0 to 75 ° C.
- the binder removal treatment and the sintering heat treatment may be performed continuously or independently.
- the atmosphere is changed without cooling, and then the temperature is raised to the holding temperature during firing, and firing is performed.
- the temperature is raised in a N 2 gas or humidified N 2 gas atmosphere to the holding temperature during debinding treatment, and then the atmosphere is changed to further raise the temperature.
- the end faces of the sintered body (element body 4) thus obtained are polished by, for example, barrel polishing, sand plasting, or the like, and the terminal electrode paint is baked to form the terminal electrodes 6, 8.
- the firing conditions for the terminal electrode coating material are preferably, for example, about 10 minutes to 1 hour at 600 to 800 ° C. in a humidified mixed gas of N 2 and H 2 .
- a pad layer is formed by plating or the like on the terminal electrodes 6 and 8 as necessary.
- the terminal electrode paint may be prepared in the same manner as the above-mentioned electrode paint.
- the multilayer ceramic capacitor of the present invention thus manufactured is mounted on a printed circuit board or the like by soldering or the like, and is used for various electronic devices and the like. [0 1 0 0]
- Dielectric paint green sheet ⁇ paint
- green sheet according to the present embodiment
- a polybutyl acetal resin having a specific range of the degree of polymerization, a specific range of the degree of petitialization, and a residual acetyl group content of a predetermined value or less is used as a binder. Therefore, even if the green sheet 10a is extremely thin, for example, about 5 or less, the green sheet 10a has strength enough to withstand peeling from the carrier sheet 30, and has good adhesiveness and handling properties. Further, the surface roughness of the sheet 10a is small, and the sheet 10a is excellent in stackability. Therefore, it is easy to laminate a large number of green sheets 10a via the electrode layers 12a, and it is possible to omit the adhesive layer 28 if necessary.
- the dispersant of a specific type and the HLB is used in a specific range. ing. Therefore, even if the green sheet 10a is extremely thin, for example, about 5 ⁇ or less, the green sheet 10a has strength enough to withstand peeling from the carrier sheet 30 and has good adhesiveness and handling properties. Further, the surface roughness of the sheet 10a is small, and the sheet 10a is excellent in stackability. Therefore, it is easy to laminate a large number of green sheets 10a via the electrode layer 12a, and it is possible to omit the adhesive layer 28 if necessary.
- the dielectric paint contains a charging aid, and the charging aid is imidazoline-based. It is an antistatic agent. Therefore, even if the green sheet 10a is extremely thin, for example, about 5 ⁇ or less, it has strength enough to withstand peeling from the carrier sheet 30 as a support, It is possible to produce a green sheet 10a that suppresses the generated static electricity and has good adhesive and handling properties. Further, the sheet 10a has a small surface roughness and is excellent in stackability. Therefore, it is easy to laminate a large number of Darling sheets 10a via the electrode layers 12a, and it is also possible to omit the adhesive layer 28 if necessary.
- the dry type electrode layer 12a can be easily formed on the surface of the green sheet 10a with high precision without the green sheet 10a being broken or deformed. In addition, it is possible to transfer with high accuracy.
- the adhesive layer 28 is formed on the surface of the electrode layer or the green sheet by a transfer method, and the electrode layer 12a is attached to the green sheet 10 via the adhesive layer 28. Adhere to the surface of a.
- the formation of the adhesive layer 28 eliminates the need for high pressure and heat when bonding and transferring the electrode layer 12a to the surface of the green sheet 10a, so that bonding at lower pressure and lower temperature is not required. Will be possible. Therefore, even when the green sheet 10a is extremely thin, the green sheet 10a is not destroyed, and the electrode layer 12a and the green sheet 10a can be satisfactorily laminated. No short circuit failure occurs.
- the adhesive force of the adhesive layer 28 is made stronger than the adhesive force of the release layer 22, and the adhesive force of the release layer 22 is also increased by the adhesive force between the green sheet 10 a and the carrier sheet 30.
- the carrier sheet 30 on the green sheet 10a side can be selectively and easily peeled off.
- the adhesive layer 28 is not formed directly on the surface of the electrode layer 12a or the green sheet 10a by a coating method or the like, but is formed by a transfer method.
- the components of the adhesive layer 28 do not permeate the electrode layer 12a or the green sheet 10a, and an extremely thin adhesive layer 28 can be formed.
- the thickness of the bonding layer 28 can be reduced to about 0.02 to 0.3 ⁇ . Even though the thickness of the adhesive layer 28 is small, the components of the adhesive layer 28 do not penetrate into the electrode layer 12a or the green sheet 10a, so that the adhesive strength is sufficient. Moreover, there is no possibility that the composition of the electrode layer 12a or the green sheet 10a is adversely affected.
- the method of the present invention is not limited to a method for manufacturing a multilayer ceramic capacitor, but can be applied to a method for manufacturing other multilayer electronic components.
- the accessory component additives were mixed in a ball mill to form a slurry. That is, the auxiliary component additive (a total amount of 8.8 g) and a solvent (16 g) containing ethanol / n-propanol in a ratio of 1: 1 were pre-milled by a ball mill for 20 hours.
- the polymerization degree of the polybutyral resin as the pinda resin was 1,400, the degree of butyralization was 69 ⁇ 3%, and the amount of residual acetyl group was 3 ⁇ 2%.
- This binder resin was contained in the ceramic paint in an amount of 6 parts by mass based on 100 parts by mass of the ceramic powder (including the ceramic powder auxiliary component additive). If the total volume of ceramic powder, binder resin, and plasticizer in the ceramic paint is 100% by volume, the volume ratio of ceramic powder is 67.31 volumes. /. Met.
- DOP as a plasticizer was contained in the ceramic paint in 50 parts by mass with respect to 100 parts by mass of the binder resin. Water was contained at 2 parts by mass based on 100 parts by mass of the ceramic powder. The polyethylene glycol-based nonionic dispersant as a dispersant was contained in 0.7 parts by mass with respect to 100 parts by mass of the ceramic powder.
- the paint contains an alcohol-based solvent and an aromatic-based solvent as solvents, and the total mass of the alcohol-based solvent and the aromatic-based solvent is 100 parts by mass, and toluene as an aromatic-based solvent is 15 parts by mass. Parts by weight were included.
- the viscosity of the paint was 180 mPa ⁇ S.
- the viscosity of the paint was measured using a B-type viscometer, using S21 as a rotor, at a measurement temperature of 25 ° C, and immediately after the paint was dropped. The measurement speed was 50 rpm.
- the paint obtained as described above was applied to a PET film as a supporting film with a thickness of 2 ⁇ by a wire bar coater, and dried to produce a green sheet.
- the coating speed was 5 OmZin i ⁇
- the drying conditions were a temperature in the drying oven of 60 ° C to 70 ° C, and a drying time of 2 minutes.
- the sheet density was determined by measuring the thickness of the sheet after drying, measuring the weight of the sheet, and dividing the weight of the sheet by the volume.
- the average surface roughness Rz was measured using a surface roughness measuring device manufactured by Kosaka Laboratory Co., Ltd.
- Sheet tensile strength and sheet elongation were measured using an Instron 5543 tensile tester, five samples of dumbbell-shaped sheets were prepared as samples, and each sample was pulled at a pulling speed of 8 Zmin and broken. The strength and elongation at the time were calculated, and the average value was calculated.
- the adhesion was evaluated as follows. First, 10 samples were prepared by cutting the dried sheet into 50 mm X 15 ram, and five sets of two sheets (temporary stack) were prepared. Each set of sheets was preheated at 70 ° C. for 5 minutes and bonded at 70 ° C. for 1 minute at about 2 MPa. Thereafter, a double-sided tape was applied to the surface of each set of sheets, and each set of sheets was pulled in the direction of peeling using a tensile tester of Instron 5543, and the peel strength at the time of peeling was measured. The higher the peel strength, the better the adhesion.
- the sheet density is 3.3 g / cm 3 or more, the surface roughness is 0.6 ⁇ or less, the sheet tensile strength is 6.OMPa or more, the sheet elongation is 37% or more, and the adhesiveness
- a sample having a peel strength of 1 ONZcm 2 or more was judged as good ( ⁇ ), and one that did not satisfy the condition was judged as bad (X).
- * in front of the numbers in the table indicates that the value is outside the preferred range. The same applies to the following table.
- a green sheet was prepared in the same manner as in Example 1 except that polyvinyl acetal resin (PVAc) of product number BX-1 manufactured by Sekisui Chemical Co., Ltd. was used as the binder resin, and the same evaluation was performed. Table 1 shows the results.
- PVAc polyvinyl acetal resin
- a green sheet was prepared and evaluated in the same manner as in Example 1, except that an acrylic resin (MMA-BA) having a molecular weight of 450,000 and a Tg of 70 ° C was used as the pinda resin. Table 1 shows the results.
- MMA-BA acrylic resin having a molecular weight of 450,000 and a Tg of 70 ° C
- PVB polybutylbutyral resin
- a green sheet was prepared in the same manner as in Example 1 except that the resin number (grade) manufactured by Sekisui Chemical Co., Ltd. was different and the degree of polymerization was 300 to 2400 as the polybutylal resin. It was fabricated and subjected to the same evaluation. Table 2 shows the results.
- the degree of polymerization of the polybutyral resin was preferably from 100 to 170. If the degree of polymerization is too low, the sheet tensile strength tends to decrease, and if the degree of polymerization is too high, the sheet density decreases, the sheet surface roughness deteriorates, and the sheet elongation and the adhesiveness also tend to decrease. That was confirmed.
- Example 1 was the same as Example 1 except that the product number (grade) manufactured by Sekisui Chemical Co., Ltd. was different and the degree of petitialization was 65 to 78 as the polybutylal resin.
- a green sheet was prepared in the same manner, and the same evaluation was performed. Table 3 shows the results.
- the degree of butyralization of the polybutyral resin was preferably 65% or more and less than 78%. It was confirmed that if the degree of petitialization is too low, the sheet elongation tends to decrease, and if it is too high, the sheet surface roughness tends to deteriorate.
- the residual acetyl group content of the polybutyral resin was preferably less than 6%.
- the residual acetyl group content was too large, it was confirmed that the sheet density was reduced, the surface roughness was increased, and the adhesiveness was likely to be reduced.
- the addition mass ratio (PHP) of the polybutyral resin as the binder resin to 100 parts by mass of the ceramic powder is preferably from 5 parts by mass to 6.5 parts by mass. did it. It was confirmed that when the mass ratio was too low, the tensile strength, the sheet elongation and the adhesiveness were reduced, and when the mass ratio was too high, the sheet density was reduced and the surface roughness was likely to be increased.
- the volume ratio occupied by the ceramic powder was preferably not less than 64.3% and not more than 72%. did it.
- the volume ratio is too low, the sheet density decreases and the surface roughness increases.
- the volume ratio is too high, the tensile strength, the sheet elongation, and the adhesiveness tend to decrease.
- dibutyl phthalate (DBP) or benzyl butyl phthalate (BBP) was used as a plasticizer, and the mass ratio (PHR) of the plasticizer was calculated based on 100 parts by mass of the pinda resin.
- a green sheet was prepared and evaluated in the same manner as in Example 1, except that the amount was changed in the range of 30 to 100 parts by mass. Table 6 shows these results.
- the ninth embodiment is the same as the first embodiment.
- the addition mass ratio is preferably from 40 parts by mass to 70 parts by mass. If the mass ratio is too low, the sheet elongation and adhesiveness decrease, and if the mass ratio is too high, the sheet density decreases, the surface roughness increases, and the tensile strength tends to decrease. Was.
- Example 13 is the same as Example 1.
- the added mass ratio of water is preferably 1 part by mass or more and 6 parts by mass or less. It was confirmed that when the mass ratio was too low, the filtration characteristics tended to deteriorate, and when the mass ratio was too high, the sheet density decreased and the surface roughness tended to increase.
- Example 8 As shown in Table 8, the same procedure as in Example 1 was performed except that the addition ratio of mineral spirit (PHP) was changed within a range of 1 to 20 parts by mass with respect to 100 parts by mass of the ceramic powder. To produce a green sheet, and the same evaluation was performed.
- PHP mineral spirit
- Example 19 Mineral Spirit 3 190 3.45 0.57 8.3 42 12.4 20
- Example 20 Mineral Spirit 5 180 3.4 0.55 8.2 49 14.5 o
- Example 21 Mineral Spirit 10 180 3.32 0.54 7.7 51 17.3 o
- Example 22 Mineral spirit 15 170 3.3 0.55 7.4 55 20.3 ⁇ Reference example 24 Mineral spirit 20 180 * 3.21 0.60.61 6.5 47 22.3 X
- the total mass of the alcohol solvent (ethanol and propanol) and the aromatic solvent (toluene) was 100 parts by mass, and the addition mass ratio of the aromatic solvent (toluene) was A green sheet was prepared in the same manner as in Example 1 except that the amount was changed in the range of 5 to 50 parts by mass, and the same evaluation as in Examples 12 to 15 was performed. Table 9 shows the results.
- the embodiment 24 is the same as the embodiment 1.
- the solvent in the paint contains an alcohol-based solvent and an aromatic-based solvent, and the total weight of the alcohol-based solvent and the aromatic-based solvent is 100 parts by mass. However, it was confirmed that the content was preferably from 10 parts by mass to 20 parts by mass. If the mass ratio is too low, the surface roughness tends to increase and the adhesiveness tends to deteriorate.If the mass ratio is too high, the filtration characteristics deteriorate, the sheet density decreases, and the surface roughness increases. It was confirmed that the tensile strength also tended to decrease.
- the binder resin was previously dissolved and filtered in at least one or more alcoholic solvents of methanol, ethanol, propanol, and butanol to form a solution. It was confirmed that it is preferable to add other components. Otherwise, it was confirmed that the filtration characteristics deteriorated and the surface roughness also tended to increase.
- Example 1b Polyethylene glycol HLB 5-6 0.7 180 3.4 0.55 8.2 49 14.5 2.25 ⁇ Example 1c Polyethylene glycol HLB 6-7 0.7 220 * 3.25 * 0.66 6J 42 15.3 X
- Example 1e Maleic acid 0.7 250 3.41 0.51 6.5 * 32 16.5 X
- the sheet density was 3.3 g cni 3 or more, the surface roughness was 0.6 / im or less, the sheet tensile strength was 6.OMPa or more, and the sheet elongation was 37%.
- the adhesive peel strength is 8.9 N / cm 2 or more, and the filtration rate
- a green sheet was prepared in the same manner as in Example 1b, except that the content of the dispersant was changed in the range of 0.2 to 2 parts by mass with respect to 100 parts by mass of the ceramic powder. Was done. The results are shown in Table 12.
- Table 12 (Amount of dispersant) Dispersant type Dispersant Sheet density table if roughness Tensile strength sheet elongation Adhesion Filtration ⁇ Judgment
- Example 1i ⁇ 0.5 220 3.35 0.58 8.3 53 14.2 4.12 ⁇ ⁇
- Example 1j ⁇ 0.7 180 3.4 0.55 8.2 49 14.5 2.25 ⁇
- Example 1k ⁇ 1 130 3.58 0.49 7.6 45 10.3 1.4 ⁇
- Example 11 ⁇ 1.5 100 3.63 0.46 6.9 41 8.9 1.32 ⁇ ⁇
- Example 1m ⁇ 2 90 3.53 0.51 * 5.3 37 * 6.6 2.21 X
- the content of the dispersant is preferably in the range of 0.5 to 1.5 parts by mass, more preferably 0.5 to 1.0 parts by mass, based on 100 parts by mass of the ceramic powder. It was confirmed that it was within the range.
- the static electricity (charging characteristics) was evaluated as follows. That is, the measurement was performed using Nakako S55-1 Co., Ltd. immediately after the green sheet was peeled, with the distance between the green sheets being 1 cm. The measured value is a value measured 5 seconds after peeling. The smaller the generated static electricity (kV), the better. When static electricity is generated, the sheets are wrinkled, which makes it difficult to perform lamination with high accuracy.
- octadecylamine acetate was used as the amine-based surfactant
- 1-hydroxyethyl 2-alkyl imidazoline quaternary salt was used as the imidazoline-based surfactant
- polyethylene glycol-based antistatic agent was used.
- Polyethylene glycol dodecyl ether was used as the agent, and PEG400 was manufactured by NOF Corporation.
- the sheet density was 3.3 g / cm 3 or more, the surface roughness was 0.6 ⁇ or less, the sheet tensile strength was 6.OMPa or more, and the sheet elongation was 4 Those with 0% or more, adhesive peel strength of 9 cm 2 or more and static electricity of 36 or less are judged to be good ( ⁇ ), and one of them that does not satisfy the condition is defective. (X), and only the static electricity evaluation items that did not satisfy the above criteria were judged as ( ⁇ ).
- the present invention it is possible to produce a green sheet having strength enough to withstand peeling from a support and having good adhesiveness and handling properties, even for an extremely thin green sheet. It is possible to provide a green sheet paint, a green sheet, a method for producing a green sheet paint, and a method for producing a green sheet, which can be performed. Therefore, it is possible to provide a method for manufacturing an electronic component suitable for making the electronic component thinner or more multilayered.
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- Engineering & Computer Science (AREA)
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- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
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- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Producing Shaped Articles From Materials (AREA)
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP04705946A EP1593660A4 (en) | 2003-01-29 | 2004-01-28 | COATING COMPOSITION FOR GREEN FILM, MANUFACTURING METHOD, GREEN FILM, METHOD OF MANUFACTURING THEREOF, ELECTRONIC COMPONENT AND MANUFACTURING METHOD THEREFOR |
US10/543,760 US7632369B2 (en) | 2003-01-29 | 2004-01-28 | Green sheet slurry, green sheet, production method of green sheet slurry, production method of green sheet, and production method of electronic device |
JP2005504728A JP3831748B2 (ja) | 2003-01-29 | 2004-01-28 | グリーンシート用塗料、グリーンシート、グリーンシート用塗料の製造方法、グリーンシートの製造方法および電子部品の製造方法 |
Applications Claiming Priority (2)
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JP2003-020167 | 2003-01-29 | ||
JP2003020167 | 2003-01-29 |
Publications (1)
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WO2004067475A1 true WO2004067475A1 (ja) | 2004-08-12 |
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ID=32820622
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PCT/JP2004/000755 WO2004067475A1 (ja) | 2003-01-29 | 2004-01-28 | グリーンシート用塗料とその製造方法、グリーンシートとその製造方法、及び電子部品の製造方法 |
Country Status (7)
Country | Link |
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US (1) | US7632369B2 (ja) |
EP (1) | EP1593660A4 (ja) |
JP (1) | JP3831748B2 (ja) |
KR (1) | KR100720795B1 (ja) |
CN (1) | CN100478304C (ja) |
TW (1) | TW200420521A (ja) |
WO (1) | WO2004067475A1 (ja) |
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JPWO2005113208A1 (ja) * | 2004-05-20 | 2008-03-27 | Tdk株式会社 | グリーンシート、グリーンシートの製造方法、および電子部品の製造方法 |
JP2008218532A (ja) * | 2007-02-28 | 2008-09-18 | Tdk Corp | グリーンシート積層ユニット、電子部品の製造方法、および電子部品 |
CN102433088A (zh) * | 2011-08-17 | 2012-05-02 | 广东风华高新科技股份有限公司 | 一种片式多层陶瓷电容器用的粘合剂及其制备方法 |
WO2020203786A1 (ja) * | 2019-03-29 | 2020-10-08 | 積水化学工業株式会社 | セラミックグリーンシート用樹脂組成物、セラミックグリーンシート及び積層セラミックコンデンサ |
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- 2004-01-28 CN CNB2004800088197A patent/CN100478304C/zh not_active Expired - Fee Related
- 2004-01-28 US US10/543,760 patent/US7632369B2/en not_active Expired - Fee Related
- 2004-01-28 JP JP2005504728A patent/JP3831748B2/ja not_active Expired - Lifetime
- 2004-01-28 EP EP04705946A patent/EP1593660A4/en not_active Withdrawn
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JPWO2005113208A1 (ja) * | 2004-05-20 | 2008-03-27 | Tdk株式会社 | グリーンシート、グリーンシートの製造方法、および電子部品の製造方法 |
JP4506755B2 (ja) * | 2004-05-20 | 2010-07-21 | Tdk株式会社 | グリーンシート、グリーンシートの製造方法、および電子部品の製造方法 |
JP2008218532A (ja) * | 2007-02-28 | 2008-09-18 | Tdk Corp | グリーンシート積層ユニット、電子部品の製造方法、および電子部品 |
CN102433088A (zh) * | 2011-08-17 | 2012-05-02 | 广东风华高新科技股份有限公司 | 一种片式多层陶瓷电容器用的粘合剂及其制备方法 |
WO2020203786A1 (ja) * | 2019-03-29 | 2020-10-08 | 積水化学工業株式会社 | セラミックグリーンシート用樹脂組成物、セラミックグリーンシート及び積層セラミックコンデンサ |
JP6821094B1 (ja) * | 2019-03-29 | 2021-01-27 | 積水化学工業株式会社 | セラミックグリーンシート用樹脂組成物、セラミックグリーンシート及び積層セラミックコンデンサ |
CN113646380A (zh) * | 2019-03-29 | 2021-11-12 | 积水化学工业株式会社 | 陶瓷生片用树脂组合物、陶瓷生片及层叠陶瓷电容器 |
Also Published As
Publication number | Publication date |
---|---|
EP1593660A1 (en) | 2005-11-09 |
EP1593660A4 (en) | 2009-01-21 |
KR20050099984A (ko) | 2005-10-17 |
CN100478304C (zh) | 2009-04-15 |
TWI320034B (ja) | 2010-02-01 |
TW200420521A (en) | 2004-10-16 |
US20060096692A1 (en) | 2006-05-11 |
US7632369B2 (en) | 2009-12-15 |
CN1768017A (zh) | 2006-05-03 |
KR100720795B1 (ko) | 2007-05-23 |
JP3831748B2 (ja) | 2006-10-11 |
JPWO2004067475A1 (ja) | 2006-05-18 |
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