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WO2011016442A1 - Pâte de dispersion de microparticules inorganiques - Google Patents

Pâte de dispersion de microparticules inorganiques Download PDF

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Publication number
WO2011016442A1
WO2011016442A1 PCT/JP2010/063075 JP2010063075W WO2011016442A1 WO 2011016442 A1 WO2011016442 A1 WO 2011016442A1 JP 2010063075 W JP2010063075 W JP 2010063075W WO 2011016442 A1 WO2011016442 A1 WO 2011016442A1
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WO
WIPO (PCT)
Prior art keywords
inorganic fine
fine particle
dispersed paste
meth
fine particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2010/063075
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English (en)
Japanese (ja)
Inventor
山内健司
宮崎寛子
麻生隆浩
杉田大平
高橋英之
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Sekisui Chemical Co Ltd
Original Assignee
Sekisui Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sekisui Chemical Co Ltd filed Critical Sekisui Chemical Co Ltd
Priority to CN201080034292.0A priority Critical patent/CN102471541B/zh
Publication of WO2011016442A1 publication Critical patent/WO2011016442A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/10—Esters
    • C08F120/12—Esters of monohydric alcohols or phenols
    • C08F120/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F120/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/40—Glass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08—Cellulose derivatives
    • C08L1/26—Cellulose ethers
    • C08L1/28—Alkyl ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of 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; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
    • C08L33/08—Homopolymers or copolymers of acrylic acid esters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate

Definitions

  • the present invention relates to an inorganic fine particle dispersed paste capable of forming a sintered layer excellent in surface smoothness.
  • an inorganic fine particle dispersed paste in which inorganic fine particles such as conductive powder and ceramic powder are dispersed in a binder resin has been used to obtain sintered bodies having various shapes.
  • phosphor pastes in which phosphors are dispersed as inorganic fine particles in a binder resin and glass pastes in which low-melting-point glass is dispersed are used in plasma display panels and the like, and demand is increasing in recent years.
  • a ceramic paste in which barium titanate or alumina as inorganic fine particles is dispersed in a binder resin is formed into a green sheet and used for a multilayer electronic component such as a multilayer ceramic capacitor.
  • the back electrode of the solar cell panel is usually formed by applying a paste in which aluminum powder is dispersed by screen printing or the like, drying, and firing.
  • the dielectric layer of a plasma display panel can be obtained by printing a glass paste on a glass substrate, drying the solvent in a blowing oven circulated through the furnace, and then degreasing and firing in a high-temperature oven. It is formed.
  • a glass paste for forming a dielectric layer for example, Patent Document 1 discloses a composition for a dielectric layer of a plasma display panel, a glass frit containing at least a glass component, a dispersant, and a pyrolysis binder. And a solvent, and the dispersant is a polycarboxylic acid polymer compound, and the dielectric layer composition is applied onto a support and then dried. The resulting green sheet is disclosed.
  • Patent Document 1 describes that the dispersion state of the glass frit is effectively improved in the dielectric layer composition described in the same document. Such improvement of the dispersibility of the inorganic fine particles is important in order to form a uniform sintered layer and not cause variations in the characteristics of the sintered layer. However, since the sintered layer is formed only after the printing, drying, degreasing, and firing steps of the inorganic fine particle dispersed paste, simply improving the uniformity in the paste state, that is, the dispersibility of the inorganic fine particles, is the final. It is difficult to ensure sufficient uniformity of the sintered layer formed on the substrate.
  • An object of this invention is to provide the inorganic fine particle dispersion
  • the present invention is an inorganic fine particle dispersed paste containing at least one selected from the group consisting of ethyl cellulose, (meth) acrylic resin and polyvinyl acetal resin, an organic compound, inorganic fine particles, and an organic solvent,
  • the organic compound is an inorganic fine particle-dispersed paste having one or more hydroxyl groups and having a normal temperature solid and a boiling point of less than 300 ° C.
  • a high boiling point solvent is used in the inorganic fine particle dispersed paste for forming a sintered layer in order to ensure printability. Furthermore, in order to dry a high boiling point solvent efficiently and to improve productivity, the ventilation oven is used in the drying process after printing.
  • the inventors of the present invention caused surface roughness in the coating layer of the inorganic fine particle dispersed paste due to air blowing in the oven, resulting in reduced surface smoothness of the sintered layer and deteriorated performance of the sintered layer. I found out.
  • the present inventors have at least one hydroxyl group in addition to at least one selected from the group consisting of ethyl cellulose, (meth) acrylic resin and polyvinyl acetal resin, inorganic fine particles and organic solvent, and
  • the inorganic fine particle dispersion paste containing an organic compound having a boiling point of less than 300 ° C. is well-dried in the drying process after printing, and the surface is roughened by receiving air in the oven when drying in the oven. It was found that the film can be uniformly dried without causing a skinning phenomenon caused by the entanglement of the resin. Furthermore, the present inventors have found that a sintered layer formed using the inorganic fine particle dispersed paste is excellent in surface smoothness, and have completed the present invention.
  • the inorganic fine particle-dispersed paste of the present invention contains at least one selected from the group consisting of ethyl cellulose, (meth) acrylic resin, and polyvinyl acetal resin.
  • the ethyl cellulose is not particularly limited, and a grade may be appropriately selected according to the printing method of the obtained inorganic fine particle dispersed paste, the desired thickness of the sintered layer, and the like. In particular, when screen printing is performed, ethyl cellulose having thixotropy is generally preferable, and grades of ethyl cellulose such as STD45 and STD100 are preferable.
  • the (meth) acrylic resin is not particularly limited as long as it decomposes at a low temperature of about 350 to 400 ° C., but methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, n-butyl (meth) ) Acrylate, tert-butyl (meth) acrylate, isobutyl (meth) acrylate, cyclohexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, isobornyl (meth) acrylate, n-stearyl (meth) acrylate, benzyl (meth) acrylate And a polymer comprising at least one selected from the group consisting of (meth) acrylic monomers having a polyoxyalkylene structure is preferred.
  • (meth) acrylate means acrylate or methacrylate.
  • polymethyl methacrylate polymer of methacrylate, Tg 105 ° C.
  • Tg glass transition temperature
  • Polymethacrylate is also excellent in low temperature degreasing properties.
  • the inorganic fine particle-dispersed paste of the present invention contains an organic compound described later, a polymer having a component derived from butyl methacrylate or isobutyl methacrylate is preferable.
  • the said (meth) acrylic resin may have the segment which consists of a monomer which has a polar group.
  • the monomer having a polar group include 2-hydroxyethyl methacrylate, hydroxypropyl methacrylate, methacrylic acid, glycidyl methacrylate, glycerol monomethacrylate, and the like.
  • content of the segment derived from the monomer which has the said polar group is 20 weight% or less. If the content of the segment derived from the monomer having the polar group exceeds 20% by weight, thermal decomposition at low temperature is impaired, or soot is attached to the inorganic fine particles, resulting in a large amount of residual carbon in the sintered body. Sometimes it becomes. More preferably, it is 10 parts by weight or less.
  • the (meth) acrylic resin preferably has a hydrophilic functional group at the molecular end.
  • the hydrophilic functional group is not particularly limited, but is preferably a carbonyl group, an amino group, or an amide group.
  • a (meth) acrylic resin in which a highly interactive functional group such as a carbonyl group, amino group, or amide group is introduced into the ester substituent of a (meth) acrylic monomer.
  • the depolymerization of the (meth) acrylic resin is inhibited, the thermal decomposition end temperature is increased, and the thermal decomposability is extremely deteriorated.
  • one molecular end of the (meth) acrylic resin is adsorbed on the surface of the inorganic fine particles, and the other is extended to the organic solvent side, preventing re-aggregation of the inorganic fine particles and improving dispersion stability. it can.
  • the weight average molecular weight by polystyrene conversion of the said (meth) acrylic resin is not specifically limited, A preferable minimum is 5000 and a preferable upper limit is 500,000.
  • a preferable minimum is 5000 and a preferable upper limit is 500,000.
  • the weight average molecular weight is less than 5,000, the resulting inorganic fine particle dispersed paste may not have sufficient viscosity and screen printing properties may be deteriorated.
  • air is blown in an oven in a drying process after printing.
  • the surface roughness due to receiving increases the surface smoothness of the sintered layer may decrease.
  • the weight average molecular weight is more than 500,000, the adhesive strength of the obtained inorganic fine particle dispersed paste becomes too high, so that the yarn may be generated and the screen printability may be deteriorated.
  • the upper limit with the said preferable weight average molecular weight is 100,000, and a more preferable upper limit is 50000.
  • the polystyrene equivalent weight average molecular weight of the (meth) acrylic resin is preferably 10,000 to 50,000 because a clear image can be obtained during screen printing.
  • the weight average molecular weight in terms of polystyrene can be obtained by GPC measurement using, for example, a column LF-804 (manufactured by Showa Denko KK) as a column.
  • the method for producing the (meth) acrylic resin is not particularly limited.
  • the above-mentioned (meth) acrylic monomer is subjected to a free radical polymerization method under a polymerization initiator having a carbonyl group, an amino group, an amide group, or the like.
  • Copolymerization by a conventionally known method such as a living radical polymerization method, an iniferter polymerization method, an anionic polymerization method, a living anion polymerization method, or a chain transfer agent having a carbonyl group, an amino group, an amide group, etc.
  • Examples thereof include a method of copolymerizing the above-described (meth) acrylic monomer by a conventionally known method such as a free radical polymerization method, a living radical polymerization method, an iniferter polymerization method, an anion polymerization method, or a living anion polymerization method. These methods may be used independently and may use 2 or more types together.
  • a polymerization initiator having a carbonyl group, an amino group, an amide group or the like as a radical polymerization initiator, a carbonyl group, an amino group, an amide at more molecular ends. Groups and the like can be introduced. The introduction of a carbonyl group, amino group, amide group or the like only at the molecular end of the (meth) acrylic resin can be confirmed by, for example, 13 C-NMR.
  • the polyvinyl acetal resin is not particularly limited as long as it has excellent compatibility with the organic solvent described later, but is obtained by acetalizing a polyvinyl alcohol resin having a saponification degree of 80 mol% or more, It is preferable that the degree of polymerization is 1000 to 4000 and the degree of acetalization is 60 to 80 mol%.
  • the saponification degree of the polyvinyl alcohol is preferably 80 mol% or more. If the degree of saponification is less than 80 mol%, the acetalization reaction becomes difficult due to poor solubility of polyvinyl alcohol in water, and if the amount of hydroxyl groups is small, the acetalization reaction itself may be difficult. is there.
  • the degree of polymerization of the polyvinyl alcohol is preferably 1000 to 4000.
  • the polymerization degree is less than 1000, for example, when used as a material for a ceramic green sheet, the strength may be insufficient. If the degree of polymerization exceeds 4000, the solubility in water may decrease, or the viscosity of the aqueous solution may become too high, making acetalization difficult. In addition, the solution viscosity becomes too high and the coatability is lowered.
  • the polymerization degree of the said polyvinyl acetal uses the polymerization degree of polyvinyl alcohol which is a raw material at the time of synthesize
  • the polyvinyl alcohol can be obtained by saponifying a vinyl ester polymer.
  • the vinyl ester include vinyl formate, vinyl acetate, vinyl propionate, vinyl pivalate and the like, and vinyl acetate is preferable from the economical viewpoint.
  • the polyvinyl alcohol preferably contains an ⁇ -olefin in the main chain. Since the hydrogen bond strength of the polyvinyl acetal resin is weakened by the ⁇ -olefin, the viscosity stability over time can be improved, and the screen printability can be improved.
  • Examples of the ⁇ -olefin include methylene, ethylene, propylene, isopropylene, butylene, isobutylene, pentylene, hexylene, cyclohexylene, cyclohexylethylene, cyclohexylpropylene, and the like, and ethylene is particularly preferable.
  • the content of the ⁇ -olefin is preferably 1 to 20 mol%.
  • the properties of the obtained polyvinyl acetal resin are no different from those of an unmodified polyvinyl acetal resin, and when it exceeds 20 mol%, the solubility of polyvinyl alcohol in water As a result, the acetalization reaction may become difficult, and the resulting polyvinyl acetal resin may become too hydrophobic to reduce its solubility in organic solvents.
  • the polyvinyl alcohol may be copolymerized with other ethylenically unsaturated monomers as long as the effects of the present invention are not impaired.
  • ethylenically unsaturated monomers include acrylic acid, methacrylic acid, (anhydrous) phthalic acid, (anhydrous) maleic acid, (anhydrous) itaconic acid, acrylonitrile methacrylonitrile, acrylamide, methacrylamide, and trimethyl.
  • terminal-modified polyvinyl alcohol obtained by copolymerizing vinyl ester monomer such as vinyl acetate with ethylene in the presence of thiol compounds such as thiol acetic acid and mercaptopropionic acid, and saponifying it. Can do.
  • the aldehyde used in the above reaction is not particularly limited.
  • formaldehyde including paraformaldehyde
  • acetaldehyde including paraacetaldehyde
  • propionaldehyde butyraldehyde
  • amylaldehyde hexylaldehyde
  • heptylaldehyde 2-ethylhexylaldehyde
  • Examples include cyclohexyl aldehyde, furfural, glyoxal, glutaraldehyde, benzaldehyde, 2-methylbenzaldehyde, 3-methylbenzaldehyde, 4-methylbenzaldehyde, p-hydroxyaldehyde, m-hydroxyaldehyde, phenylacetaldehyde, phenylpropionaldehyde and the like.
  • These aldehydes may be used alone or in combination of two or more, and acetaldehyde and
  • the polyvinyl acetal resin is prepared by dissolving a polyvinyl alcohol resin in warm water, adding an aldehyde so as to have a predetermined degree of acetalization in the presence of an acid catalyst, reacting, and then washing, neutralizing, and drying.
  • the acid catalyst is not particularly limited, and any organic acid or inorganic acid can be used. Examples thereof include acetic acid, paratoluenesulfonic acid, nitric acid, sulfuric acid, and hydrochloric acid.
  • an alkali used for neutralization sodium hydroxide, potassium hydroxide, ammonia, sodium acetate, sodium carbonate, sodium hydrogencarbonate, potassium carbonate etc. are mentioned, for example.
  • the degree of acetalization of the polyvinyl acetal resin used in the present invention is preferably 60 to 80 mol%.
  • the degree of acetalization is less than 60 mol%, the hydrogen bondability of the polyvinyl acetal resin becomes too strong, and sufficient screen printability may not be obtained.
  • the polyvinyl acetal resin having a degree of acetalization exceeding 80 mol% is generally difficult to produce industrially.
  • the maximum acetalization degree is preferably 81.6 mol% according to the theoretical calculation by PJ Flory. J. Am. Chem. Soc., 61, 1518 (1939)).
  • the content of at least one selected from the group consisting of ethyl cellulose, (meth) acrylic resin and polyvinyl acetal resin in the inorganic fine particle-dispersed paste of the present invention is not particularly limited, but the preferred lower limit is 5% by weight and the preferred upper limit is 25. % By weight.
  • the resulting inorganic fine particle dispersed paste cannot obtain a sufficient viscosity, The screen printability may be deteriorated, and the surface smoothness of the sintered layer may be reduced due to increase in surface roughness due to receiving air blow in the oven in the drying step after printing.
  • the resulting inorganic fine particle-dispersed paste may have excessively high viscosity and adhesive strength, resulting in poor screen printability.
  • the inorganic fine particle-dispersed paste of the present invention contains an organic compound having one or more hydroxyl groups and having a normal temperature solid and a boiling point of less than 300 ° C.
  • the organic compound is solid at room temperature.
  • the resulting inorganic fine particle-dispersed paste is suppressed in surface roughness due to being blown in an oven in the drying step after printing, and the sintered layer is excellent in surface smoothness.
  • distribution paste can be obtained by melt
  • the organic compound is different from the organic solvent described later.
  • the mechanism of improving the drying property by adding an organic compound having at least one hydroxyl group and having a normal temperature solid and a boiling point of less than 300 ° C. is considered as follows.
  • the surface of the inorganic fine particles added to the inorganic fine particle-dispersed paste is in a very high polarity state, and has a function of sucking high polar functional groups.
  • an organic material having a highly polar functional group is not added to the inorganic fine particle-dispersed paste, the fine particles are aggregated in a solvent to cause precipitation.
  • an organic compound having one or more hydroxyl groups and having a normal temperature solid and a boiling point of less than 300 ° C. in the inorganic fine particle dispersed paste, it becomes liquid by mixing with an organic solvent.
  • a layer capable of adsorbing preferentially on the surface of the inorganic fine particles and evaporating around the inorganic fine particles under dry conditions can be formed.
  • the organic solvent is removed from the surface of the inorganic fine particle dispersed paste under dry conditions.
  • the surface is skinned and a thin resin layer is formed.
  • the surface resin layer formed with such drying is very non-uniform, depends on the drying conditions, and forms a more non-uniform layer under strong drying conditions under blowing conditions. For this reason, the organic solvent present under the skinned resin layer is difficult to evaporate, and unevenness is likely to occur on the surface of the coating film.
  • the organic compound having a layer formed on the surface of the inorganic fine particles evaporates under dry conditions, thereby forming a window for evaporating the internal organic solvent. Therefore, it is possible to reduce the drying unevenness of the organic solvent due to resin skinning, and even when drying is inadequate, it is a solid at room temperature, so it hardly acts as a plasticizer and maintains smoothness. It becomes easy.
  • the organic compound has a boiling point of less than 300 ° C.
  • the boiling point of the organic compound is 300 ° C. or higher, the resulting inorganic fine particle-dispersed paste has reduced drying properties in the drying step after printing, and the surface smoothness of the sintered layer is reduced.
  • the organic compound preferably has a boiling point of less than 280 ° C, more preferably less than 260 ° C.
  • the lower limit of the boiling point of the organic compound is not particularly limited, but the boiling point is preferably 160 ° C. or higher.
  • the said boiling point means the boiling point in a normal pressure.
  • the organic compound has one or more hydroxyl groups.
  • the storage stability of the resulting inorganic fine particle dispersed paste can be increased, and the viscosity of the inorganic fine particle dispersed paste can be increased by the interaction between the hydroxyl group, the resin and the organic solvent.
  • the viscosity can be made suitable for screen printing or the like.
  • the organic compound is not particularly limited as long as it has one or more hydroxyl groups and is a solid at normal temperature and has a boiling point of less than 300 ° C., but an alcohol-based organic compound composed of an aliphatic chain having 5 to 20 carbon atoms is preferable.
  • the alcohol organic compound is not particularly limited.
  • 2,2-dimethyl-1,3-propanediol, 2,2-diethyl-1,3-propanediol, 2-butyl-2-ethyl-1,3-propane which have a high ratio of hydroxyl group to carbon number
  • the diol has a boiling point of about 200 ° C. and a softening point of 120 ° C. or more, it can be suitably used as an inorganic fine particle dispersed paste used for screen printing.
  • the content of the organic compound in the inorganic fine particle-dispersed paste of the present invention is not particularly limited, but the preferred lower limit is 1% by weight and the preferred upper limit is 30% by weight.
  • the content of the organic compound is less than 1% by weight, the resulting inorganic fine particle-dispersed paste has reduced drying properties in the drying step after printing, or increased surface roughness due to receiving air blowing in the oven, The surface smoothness of the sintered layer may be reduced by causing a skinning phenomenon caused by the entanglement of the resin.
  • the content of the organic compound exceeds 30% by weight, the obtained inorganic fine particle-dispersed paste may have poor storage stability.
  • the inorganic fine particle dispersed paste of the present invention contains an organic solvent.
  • the organic solvent is not particularly limited, for example, ethylene glycol ethyl ether, ethylene glycol monobutyl ether, ethylene glycol monoethyl ether acetate, diethylene glycol monoethyl ether, diethylene glycol monomethyl ether, diethylene glycol monoisobutyl ether, trimethylpentanediol monoisobutyrate, Butyl carbitol, butyl carbitol acetate, texanol, isophorone, butyl lactate, dioctyl phthalate, dioctyl adipate, benzyl alcohol, phenylpropylene glycol, cresol, terpineol, terpine acetate, dihydroterpineol, dihydroterpineol acetate, acetone, methyl ethyl ketone, methanol, Ethan
  • the content of the organic solvent in the inorganic fine particle-dispersed paste of the present invention is not particularly limited, but a preferred lower limit is 10% by weight and a preferred upper limit is 60% by weight.
  • a preferred lower limit is 10% by weight
  • a preferred upper limit is 60% by weight.
  • the content of the organic solvent is less than 10% by weight, the viscosity and adhesive strength of the resulting inorganic fine particle-dispersed paste may become too high, resulting in poor screen printability.
  • the content of the organic solvent exceeds 60% by weight, the resulting inorganic fine particle-dispersed paste may not have a sufficient viscosity and may have poor screen printability.
  • the surface smoothness of the sintered layer may decrease due to a decrease in surface roughness or an increase in surface roughness due to receiving air blow in the oven.
  • the inorganic fine particle dispersion paste of this invention it is preferable to bake in the state which dried the said organic solvent and organic compound. If the organic solvent or organic compound is insufficiently dried, and baking is performed in a state where the organic solvent or organic compound remains in the interior, soot generated by thermal decomposition of the binder resin is likely to be adsorbed on the surface of the fine particles. Compared with the case of complete drying, the carbon residue may be increased.
  • the inorganic fine particle dispersed paste of the present invention contains inorganic fine particles.
  • the inorganic fine particles are not particularly limited, and examples thereof include glass powder, ceramic powder, phosphor fine particles, silicon oxide, metal fine particles, metal oxide fine particles, and the like.
  • the glass powder is not particularly limited, and examples thereof include glass powders such as bismuth oxide glass, silicate glass, lead glass, zinc glass, and boron glass, CaO—Al 2 O 3 —SiO 2 series, MgO—Al 2 O, and the like. 3 -SiO 2 based glass powder or the like of the LiO 2 -Al 2 O 3 -SiO 2 system such as various silicon oxide and the like.
  • R is an element selected from the group consisting of Zn, Ba, Ca, Mg, Sr, Sn, Ni, Fe, and Mn.
  • the ceramic powder is not particularly limited, and examples thereof include alumina, zirconia, titanium oxide, barium titanate, alumina nitride, silicon nitride, and boron nitride.
  • nano-ITO used for a transparent electrode material, nano-titanium oxide used for a dye-sensitized solar cell, etc. can be used suitably.
  • the phosphor fine particles are not particularly limited, and examples thereof include BaMgAl 10 O 17 : Eu, Zn 2 SiO 4 : Mn, (Y, Gd) BO 3 : Eu, and the like.
  • the metal fine particles are not particularly limited, and examples thereof include powders made of nickel, palladium, platinum, gold, silver, aluminum, tungsten, alloys thereof, and the like. Further, metals such as copper and iron, which have good adsorption characteristics with a carboxyl group, amino group, amide group and the like and are easily oxidized, can be suitably used. These metal powders may be used alone or in combination of two or more.
  • content of the said inorganic fine particle in the inorganic fine particle dispersion paste of this invention is not specifically limited, A preferable minimum is 20 weight% and a preferable upper limit is 90 weight%.
  • a preferable minimum is 20 weight% and a preferable upper limit is 90 weight%.
  • the content of the inorganic fine particles is less than 20% by weight, the obtained inorganic fine particle-dispersed paste cannot obtain a sufficient viscosity and screen printing properties may be deteriorated.
  • the surface smoothness of the sintered layer may be reduced by increasing the surface roughness due to receiving air in the interior. If the content of the inorganic fine particles exceeds 90% by weight, the resulting inorganic fine particle-dispersed paste may have too high a viscosity and screen printing properties may deteriorate.
  • the inorganic fine particle-dispersed paste of the present invention preferably contains a surfactant in order to stabilize the compatibility between the organic compound and other materials.
  • the surfactant is not particularly limited, but a nonionic surfactant is preferable.
  • content of the said nonionic surfactant in the inorganic fine particle dispersion paste of this invention is not specifically limited, A preferable upper limit is 5 weight%.
  • the nonionic surfactant has good thermal decomposability, if the content exceeds 5% by weight, the thermal decomposability of the inorganic fine particle dispersed paste may be lowered.
  • the method for producing the inorganic fine particle-dispersed paste of the present invention is not particularly limited, and examples thereof include conventionally known stirring methods. Specifically, for example, selected from the group consisting of ethyl cellulose, (meth) acrylic resin, and polyvinyl acetal resin. And a method in which at least one of the above-mentioned organic compound, the above-mentioned organic solvent, the above-mentioned inorganic fine particles, and other components added as necessary are stirred with a three-roll or the like.
  • the inorganic fine particle-dispersed paste of the present invention is well dried in the drying step after printing, the surface roughness due to receiving air blow in the oven is suppressed, and the adverse effect of the skinning phenomenon during drying can be prevented.
  • a sintered layer having excellent surface smoothness can be formed. Therefore, for example, suitable as glass paste when glass powder is used as inorganic fine particles, ceramic paste when ceramic powder is used as inorganic fine particles, and conductive paste when metal such as aluminum or conductive powder is used as inorganic fine particles Used for.
  • glass paste when glass powder is used as the inorganic fine particles is preferably used for forming a dielectric layer of a plasma display panel.
  • a glass dielectric produced using such a glass paste is also one aspect of the present invention.
  • the inorganic fine particle-dispersed paste of the present invention is characterized in that it can be dried quickly while preventing the skinning phenomenon during drying. Therefore, when a conventional resin paste is used, it can be suitably used for a member that is difficult to maintain its shape by flowing during drying. The state where the shape cannot be maintained is also referred to as “sag”. For example, when a conventional resin paste is used for the phosphor in the cell on the back plate of the plasma display, the surface electrode of the solar battery cell, etc., it drew during drying and the height could not be maintained after printing.
  • a flat panel display produced using the inorganic fine particle dispersed paste of the present invention is also one aspect of the present invention.
  • distribution paste which can form the sintered layer excellent in surface smoothness can be provided.
  • Polymerization example 1 100 parts by weight of isobutyl methacrylate (IBMA) and 100 parts by weight of texanol as an organic solvent were mixed in a 2 L separatory flask equipped with a stirrer, a cooler, a thermometer, an oil bath, and a nitrogen gas inlet to obtain a monomer mixture. .
  • IBMA isobutyl methacrylate
  • texanol as an organic solvent
  • the obtained monomer mixture was bubbled with nitrogen gas for 20 minutes to remove dissolved oxygen, and then the temperature inside the separable flask system was replaced with nitrogen gas and heated up until the oil bath reached 130 ° C. while stirring. .
  • a polymerization initiator a solution in which 2,2'-azobis [2-methyl-N- (2-hydroxyethyl) propionamide] was dispersed with texanol was added. Further, a texanol solution containing a polymerization initiator was added several times during the polymerization, and 1.5 parts by weight of the polymerization initiator was added to 100 parts by weight of the monomer in total.
  • Polymerization example 2 In a 2 L separate flask equipped with a stirrer, cooler, thermometer, oil bath, and nitrogen gas inlet, 100 parts by weight of a 1: 1 mixture of butyl methacrylate and methyl methacrylate (BMA / MMA), texanol as an organic solvent 100 parts by weight were mixed to obtain a monomer mixture.
  • BMA / MMA butyl methacrylate and methyl methacrylate
  • the obtained monomer mixture was bubbled with nitrogen gas for 20 minutes to remove dissolved oxygen, and then the temperature inside the separable flask system was replaced with nitrogen gas and heated up until the oil bath reached 130 ° C. while stirring. .
  • a polymerization initiator a solution in which 2,2'-azobis [2-methyl-N- (2-hydroxyethyl) propionamide] was dispersed with texanol was added. Further, a texanol solution containing a polymerization initiator was added several times during the polymerization, and 1.5 parts by weight of the polymerization initiator was added to 100 parts by weight of the monomer in total.
  • the obtained monomer mixture was bubbled with nitrogen gas for 20 minutes to remove dissolved oxygen, and then the temperature inside the separable flask system was replaced with nitrogen gas and heated up until the oil bath reached 130 ° C. while stirring. .
  • a solution in which azobisisobutyronitrile was dispersed with terpineol as a polymerization initiator was added. Further, a terpineol solution containing a polymerization initiator was added several times during the polymerization, and 0.8 parts by weight of the polymerization initiator was added to 100 parts by weight of the monomer in total.
  • the obtained monomer mixture was bubbled with nitrogen gas for 20 minutes to remove dissolved oxygen, and then the temperature inside the separable flask system was replaced with nitrogen gas and heated up until the oil bath reached 130 ° C. while stirring. .
  • a solution in which azobisisobutyronitrile was dispersed with terpineol as a polymerization initiator was added. Further, a terpineol solution containing a polymerization initiator was added several times during the polymerization, and 1.5 parts by weight of the polymerization initiator was added to 100 parts by weight of the monomer in total.
  • the obtained monomer mixture was bubbled with nitrogen gas for 20 minutes to remove dissolved oxygen, and then the temperature in the separable flask system was replaced with nitrogen gas and heated until the water bath boiled while stirring.
  • a polymerization initiator 0.1 part by weight of an organic oxide polymerization catalyst (Perloyl 355, manufactured by NOF Corporation) was added, a polymerization initiator was added several times during the polymerization, and the total was 100 parts by weight of the monomer. 1.5 parts by weight of a polymerization initiator was added.
  • Example 1 Ethylcellulose STD4 was dissolved in terpineol. To this terpineol solution, 1,6-hexanediol was added as an organic compound so that the composition ratio shown in Table 1 was obtained, and a vehicle composition was obtained.
  • BL-4.2 manufactured by Nikko Chemical Co., Ltd.
  • glass fine particles having an average particle size of 2.0 ⁇ m as inorganic fine particles SiO 2 32.5%, B 2 O 3 and 20.5% ZnO and 18% Al 2 O 3 10%, 3.5% and BaO, 9% of Li 2 O, 6% of Na 2 O, the SnO 2 0.5% Content
  • SiO 2 32.5%, B 2 O 3 and 20.5% ZnO and 18% Al 2 O 3 10%, 3.5% and BaO, 9% of Li 2 O, 6% of Na 2 O, the SnO 2 0.5% Content was added so as to have the composition ratio shown in Table 1, and then sufficiently kneaded using a high-speed stirrer and processed until it became smooth with a three-roll mill to prepare an inorganic fine particle-dispersed paste.
  • Example 2 Dispersion of inorganic fine particles in the same manner as in Example 1, except that ethylcellulose STD45 was used instead of ethylcellulose STD4, myristyl alcohol was used instead of 1,6-hexanediol as the organic compound, and the composition ratio was changed to the composition shown in Table 1. A paste was prepared.
  • Example 3 Except that the texanol solution of (meth) acrylic resin (Poly (IBMA)) obtained in Polymerization Example 1 was used instead of the terpineol solution of ethyl cellulose STD4, the composition ratio was changed to the composition ratio shown in Table 1, and the same as in Example 1 Thus, an inorganic fine particle-dispersed paste was prepared.
  • Example 4 Example 1 except that the texanol solution of (meth) acrylic resin (Poly (BMA / MMA)) obtained in Polymerization Example 2 was used instead of the terpineol solution of ethyl cellulose STD4 and the composition ratio was changed to that shown in Table 1. In the same manner, an inorganic fine particle dispersed paste was prepared.
  • Example 5 (Synthesis of polyvinyl acetal resin) 193 g of polyvinyl alcohol having a polymerization degree of 1700 and a saponification degree of 98 mol% was added to 2900 g of pure water and stirred at a temperature of 90 ° C. for about 2 hours for dissolution. This solution is cooled to 40 ° C., 20 g of hydrochloric acid having a concentration of 35% by weight and 145 g of n-butyraldehyde are added thereto, the temperature of the solution is lowered to 15 ° C., and this temperature is maintained to conduct an acetalization reaction. The product was precipitated. Thereafter, the liquid temperature was kept at 40 ° C.
  • polyvinyl acetal resin was dissolved in DMSO-d 6 (dimethyl sulfoxide), and the degree of acetalization was measured using 13 C-NMR (nuclear magnetic resonance spectrum). The degree of acetalization was 78 mol%. there were.
  • Example 6 To the terpineol solution of the (meth) acrylic resin (Poly (BMA / HEMA)) obtained in Polymerization Example 3, terpineol was added and dissolved so as to have the composition ratio described in Table 1. To this, 2,2-dimethyl-1,3-propanediol as an organic compound was further added so as to have the composition ratio shown in Table 1, and dispersed with a high-speed disperser. Further, aluminum fine particles (average particle size of 5 ⁇ m) as conductive fine particles and low melting point glass fine particles (average particle size of 1 ⁇ m) enabling fire-through are added so as to have the composition ratio shown in Table 1, and a high-speed stirring device is added. After using and kneading sufficiently, treatment was performed with a three roll mill while paying attention not to flatten the aluminum fine particles, and a conductive fine particle dispersed paste was prepared.
  • Table 6 To the terpineol solution of the (meth) acrylic resin (Poly (BMA / H
  • Example 7 Using a solution obtained by dissolving ethyl cellulose STD4 in terpineol and a terpineol solution of (meth) acrylic resin (Poly (BMA / MMA / HEMA)) obtained in Polymerization Example 4 so as to have the composition ratio described in Table 1. An inorganic fine particle-dispersed paste was produced in the same manner as in Example 1 except that the change was made.
  • Example 8 A terpineol solution of (meth) acrylic resin (Poly (CHMA / MMA / HEMA)) obtained in Polymerization Example 5, a rosin compound (KR85, manufactured by Arakawa Chemical Co., Ltd.), and green phosphor for PDP (Zn 2 SiO) as inorganic fine particles 4 ; Mn, manufactured by Nichia Corporation), an inorganic fine particle-dispersed paste was prepared in the same manner as in Example 1 except that the composition ratio was changed to the composition ratio shown in Table 1.
  • Example 9 Table using a texanol solution of (meth) acrylic resin (Poly (CHMA / MMA / HEMA)) obtained in Polymerization Example 6, ethyl cellulose (STD7), and silver powder (particle size 2 ⁇ m, manufactured by Shoei Chemical Co., Ltd.) as inorganic fine particles.
  • An inorganic fine particle-dispersed paste was prepared in the same manner as in Example 1 except that the composition ratio was changed to the composition ratio described in 1.
  • Example 1 An inorganic fine particle-dispersed paste was prepared in the same manner as in Example 1 except that 1,6-hexanediol as an organic compound was not used and the composition ratio was changed to those shown in Table 1.
  • Example 2 An inorganic fine particle-dispersed paste was prepared in the same manner as in Example 3 except that 1,6-hexanediol as the organic compound was not used and the composition ratio was changed as shown in Table 1.
  • Example 3 An inorganic fine particle-dispersed paste was prepared in the same manner as in Example 6 except that 2,2-dimethyl-1,3-propanediol as an organic compound was not used and the composition ratio was changed as shown in Table 1.
  • Example 6 (Comparative Example 6) Instead of the organic compound 2,2-dimethyl-1,3-propanediol, the same procedure as in Example 8 was used, except that 2-methyl-1,3-propanediol having a hydroxyl group and a liquid at room temperature was used. Thus, an inorganic fine particle dispersed paste was prepared.
  • Example 7 (Comparative Example 7) Instead of the organic compound 2,2-dimethyl-1,3-propanediol, the same procedure as in Example 9 was used, except that 2-methyl-1,3-propanediol having a hydroxyl group and a liquid at room temperature was used. Thus, an inorganic fine particle dispersed paste was prepared.
  • the inorganic fine particle dispersed paste was coated on a glass substrate, dried in a blow oven at 150 ° C. for 30 minutes, and then in an electric furnace at 500 ° C. for 30 minutes. Baked. About the obtained sintered layer, residual carbon (ppm) was measured with a carbon sulfur analyzer (manufactured by Horiba Ltd.), and the baked color was visually confirmed. The case where the residual carbon was 150 ppm or less was evaluated as “ ⁇ ”, and the case where the residual carbon exceeded 150 ppm was evaluated as “X”.
  • the obtained inorganic fine particle-dispersed paste was printed on a glass substrate and dried in a blown oven set at 120 ° C. for 20 minutes. Then, the height of the printed shape was evaluated using a laser microscope. The case where the height of the printed shape after drying was 10 ⁇ m or more was designated as “ ⁇ ”, and the case where the height of the printed shape was less than 10 ⁇ m due to sagging during drying was designated as “X”.
  • distribution paste which can form the sintered layer excellent in surface smoothness can be provided.

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Abstract

L’invention concerne une pâte de dispersion de microparticules inorganiques qui peut former une couche frittée présentant un excellent lissé de surface. Ladite pâte de dispersion de microparticules inorganiques contient : au moins une espèce choisie dans un groupe comprenant l’éthylcellulose, les résines (méth)acryliques et les résines de polyvinylacétal ; un composé organique ; des microparticules inorganiques ; et un solvant organique. Le composé organique contient un ou plusieurs groupes hydroxyle, est solide à température ambiante et a un point d’ébullition inférieur à 300 °C.
PCT/JP2010/063075 2009-08-04 2010-08-03 Pâte de dispersion de microparticules inorganiques Ceased WO2011016442A1 (fr)

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JP2014224221A (ja) * 2013-04-15 2014-12-04 積水化学工業株式会社 樹脂組成物
EP3018170A1 (fr) * 2014-11-07 2016-05-11 Kusumoto Chemicals, Ltd. Liant de résine organique facilement thermo-dégradable
JP2017048061A (ja) * 2015-08-31 2017-03-09 日本電気硝子株式会社 ガラスペースト組成物及び被膜形成ガラス部材の製造方法

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CN104327550A (zh) * 2014-09-28 2015-02-04 安徽盛佳彩印包装有限公司 一种具有导电性的改性碳酸钙及其制备方法
CN104312212A (zh) * 2014-09-28 2015-01-28 安徽盛佳彩印包装有限公司 一种综合性能好耐腐蚀的改性碳酸钙及其制备方法
CN104356690A (zh) * 2014-09-28 2015-02-18 安徽省温禾木业有限公司 一种具有阻燃效果的改性碳酸钙及其制备方法
CN104387800A (zh) * 2014-09-28 2015-03-04 安徽省温禾木业有限公司 一种环保清香改性碳酸钙及其制备方法
TWI609059B (zh) * 2015-07-22 2017-12-21 昭榮化學工業股份有限公司 Inorganic particle dispersion paste, adhesive resin and inorganic particle dispersion paste
KR102172643B1 (ko) * 2017-07-25 2020-11-02 한국세라믹기술원 쿡탑 데코층 형성을 위한 페이스트 조성물 및 이를 이용한 쿡탑 데코층의 형성방법
WO2020045174A1 (fr) * 2018-08-30 2020-03-05 積水化学工業株式会社 Composition de véhicule pour dispersion de particules fines inorganiques, composition de suspension de particules fines inorganiques dispersées et procédé de production de feuille de particules fines inorganiques dispersées
CN114049986B (zh) * 2021-12-28 2022-04-19 西安宏星电子浆料科技股份有限公司 一种无铅无铋的介质浆料

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