JP2012140558A - Inorganic particle dispersion paste composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an inorganic particle dispersion paste composition having a high viscosity, being excellent in screen printability and dispense printability, and being capable of being fired at a low temperature.SOLUTION: The inorganic particle dispersion paste composition includes a gelatinous particle containing a crosslinking (meth)acrylic resin, an inorganic microparticle, and an organic solvent, wherein the gelatinous particle containing a crosslinking (meth)acrylic resin is obtained by swelling a resin microparticle containing ≥70 wt.% of the crosslinking (meth)acrylic resin with the organic solvent, and the particle diameter of the resin microparticle containing ≥70 wt.% of the crosslinking (meth)acrylic resin is ≤10 μm; and the crosslinking (meth)acrylic resin is a copolymer having a segment originated from a monofunctional (meth)acrylic monomer and a segment originated from a polyfunctional (meth)acrylic monomer.

Description

The present invention relates to an inorganic fine particle-dispersed paste composition that has a high viscosity, is excellent in screen printability and dispense printability, and can be fired at a low temperature.

Paste compositions in which inorganic fine particles such as conductive powder, conductive powder, and ceramic powder are dispersed in a resin binder are used to obtain sintered bodies having various shapes.
For example, a conductive paste in which conductive powder is dispersed in a binder resin is used for circuit formation, capacitor manufacture, and the like. Ceramic paste or glass paste in which ceramic powder or glass powder is dispersed in a binder resin is used for manufacturing a dielectric layer of a plasma display panel (PDP), a multilayer ceramic capacitor, a fluorescent display tube, or the like. Furthermore, a paste composition in which ITO in which tin oxide is doped with tin oxide is dispersed in a binder resin is used as a transparent electrode material for manufacturing a PDP, a liquid crystal display panel (LCD), a circuit formation of a solar cell panel driving unit, and the like. It is used. In addition, a paste composition in which a phosphor is dispersed in a binder resin is used in an inorganic electroluminescence (EL) element, a PDP, and a paste composition in which silver is dispersed in a binder resin is used in solar cells, LEDs, and the like. . In recent years, the demand for these inorganic fine particle-dispersed paste compositions has been rapidly increasing.

Such inorganic fine particle-dispersed paste composition is, for example, a coating method, sheet-like printing using screen printing, die coating printing, doctor blade printing, roll coating printing, offset printing, gravure printing, flexographic printing, inkjet printing, dispensing printing, etc. After processing into a predetermined shape by a casting method or the like for processing into a sintered body, a sintered body having a required shape can be obtained by firing. Of these, the screen printing method is particularly suitable for mass production. The dispense printing method is particularly suitable for precise printing, and is used for pattern formation of electronic parts.

In order to perform screen printing and dispense printing satisfactorily, the viscosity is sufficiently low during coating, and coating is easy, while the viscosity is sufficiently high when allowed to stand and dry after coating. Therefore, the paste composition preferably has a so-called thixotropic property (hereinafter also referred to as “thixotropy”). The thixotropy is, for example, when the viscosity is evaluated with a rotational viscometer, the viscosity is low when the rotational speed is high (displacement with a high strain rate), and the viscosity is low when the rotational speed is low (displacement with a low strain rate). Is a high property.

Generally, a binder resin contained in a paste composition used for screen printing or dispense printing is prepared by dissolving ethyl cellulose in a high-boiling organic solvent. Ethyl cellulose has a higher viscosity and becomes difficult to dissolve in organic solvents as the ethoxylation rate increases, but it can make the paste composition thixotropic by leaving undissolved matter of several microns without completely dissolving it. it can. That is, the ethyl cellulose particles remaining in an undissolved state in the paste composition function as a pseudo-crosslinking point, so that when the shear strain is applied to the paste composition, the stress changes according to the strain rate. When the shear rate is high, the pseudo-crosslinking points are destroyed and the viscosity of the paste composition is lowered. On the other hand, when the shear rate is low, the destruction and recovery of the pseudo-crosslinking points of the paste composition occur simultaneously. Indicates a high viscosity. Therefore, even if the blending amount of ethyl cellulose is small, the resulting paste composition has a high viscosity and hardly produces stringing.

In the coating method of the paste composition using screen printing or dispense printing, for example, the paste composition in which inorganic fine particles are dispersed in a binder resin such as ethyl cellulose is applied on the substrate by screen printing or dispensing printing, and then A layer made of inorganic fine particles is formed by sintering. However, ethyl cellulose generally used as a binder resin cannot be completely decomposed unless heated at a high temperature of 500 ° C. or higher, and metal fine particles are deteriorated by heating at a high temperature during sintering. If it was insufficient, there were problems such as deterioration of the characteristics of the metal fine particles due to residual carbon after sintering. In addition, ethyl cellulose contains a large number of impurity ions derived from natural products, and when the paste composition is used for semiconductors or the like, this impurity ion may cause a problem.

On the other hand, Patent Document 1 discloses a paste composition using a (meth) acrylic resin having good thermal decomposability. However, since (meth) acrylic resin has strong adhesiveness, when printing a paste composition using a screen printing device, the transferred paste composition is stringed and returned to the back side of the screen printing plate to print the pattern. There was a problem that a defect occurred. Moreover, when printing a paste composition using a dispense printing apparatus, there existed a problem that cells other than the cell filled with a paste composition were contaminated by the stringing of the paste composition.
Furthermore, since the (meth) acrylic resin has a relatively low viscosity, if the blending amount of the (meth) acrylic resin is increased in order to increase the viscosity of the paste composition to an extent suitable for printing, undecomposed residues during sintering If the molecular weight of the (meth) acrylic resin is increased in order to increase the viscosity of the paste composition with a small amount of (meth) acrylic resin, stringing tends to occur and it is used for screen printing and dispense printing. It was difficult.

Patent Document 2 discloses a method of blending fine particles made of a crosslinked acrylic resin into a paste composition. In Patent Document 2, even when stringing occurs in the paste composition, the fine particles made of the crosslinked acrylic resin serve as the starting point of thread breakage. However, since the fine particles comprising the crosslinked acrylic resin have a low thickening effect, a large amount of resin is required to increase the viscosity of the paste composition, and there is a problem that undecomposed residues during sintering increase.

Patent Document 3 discloses a method of blending fine particles having a core-shell structure into a paste composition. In Patent Document 3, the core portion is cross-linked, but the shell portion is not cross-linked, so that there is a problem that the particles tend to aggregate and the viscosity is not stable.

JP 2000-104053 A JP-A-10-083760 JP 2010-126560 A

An object of the present invention is to provide an inorganic fine particle-dispersed paste composition that has a high viscosity, is excellent in screen printability and dispense printability, and can be fired at a low temperature.

The present invention is an inorganic fine particle-dispersed paste composition containing a cross-linked (meth) acrylic resin, inorganic fine particles and an organic solvent, wherein the gel-like particles containing the cross-linked (meth) acrylic resin are cross-linked ( A resin fine particle containing 70% by weight or more of a (meth) acrylic resin is swollen with the organic solvent, and the particle diameter is 10 μm or less. The crosslinked (meth) acrylic resin is a monofunctional (meth) acrylic monomer. It is an inorganic fine particle dispersion paste composition which is a copolymer having a segment derived from and a segment derived from a polyfunctional (meth) acrylic monomer.
The present invention is described in detail below.

In the case of using a (meth) acrylic resin as a binder resin, the present inventors include a swollen gel containing an undissolved crosslinked (meth) acrylic resin in the paste composition, whereby the swollen gel is pseudo-crosslinked. It has been found that the point composition can increase the viscosity of the paste composition and improve the thixotropy.
However, the gel is usually in a state of being bridged from end to end of the system and is in a solid state, so that there is a problem that it is difficult to use it for paste applications.
Therefore, the present inventors have used an inorganic fine particle-dispersed paste composition that has high viscosity and can suppress stringing by using gelled particles of a crosslinked (meth) acrylic resin having a particle size of 10 μm or less as a binder resin. The present inventors have found that a product can be obtained and have completed the present invention.

The inorganic fine particle-dispersed paste composition of the present invention contains gel-like particles containing a crosslinked (meth) acrylic resin (hereinafter also simply referred to as gel-like particles). When the gel-like particles contain a crosslinked (meth) acrylic resin, the inorganic fine particle-dispersed paste composition of the present invention can produce a sintered body of inorganic fine particles with lower firing energy.

The crosslinked (meth) acrylic resin is a copolymer having a segment derived from a monofunctional (meth) acrylic monomer and a segment derived from a polyfunctional (meth) acrylic monomer.

The monofunctional (meth) acrylic monomer is not particularly limited. For example, methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, n-butyl (meth) acrylate, tert-butyl (meth) acrylate, Examples include isobutyl (meth) acrylate, cyclohexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, isobornyl (meth) acrylate, n-stearyl (meth) acrylate, and benzyl (meth) acrylate.
Moreover, you may use the (meth) acryl monomer which has a polyoxyalkylene structure for the said monofunctional (meth) acryl monomer. The polyoxyalkylene structure is not particularly limited, and examples thereof include a polyoxypropylene structure, a polyoxymethylethylene structure, a polyoxyethylethylene structure, a polyoxytrimethylene structure, and a polyoxytetramethylene structure.
Among the monofunctional (meth) acrylic monomers, methyl methacrylate is preferable because it can be decomposed at a lower temperature.
In the present specification, “(meth) acryl” means “acryl or methacryl”.

The polyfunctional (meth) acrylic monomer is not particularly limited, and examples thereof include ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, allyl (meth) acrylate, and trimethylolpropane tri (meth) acrylate.
The polyfunctional (meth) acrylate may be modified with ethylene oxide.

The preferable lower limit of the content ratio of the segment derived from the polyfunctional (meth) acrylic monomer in the crosslinked (meth) acrylic resin is 0.5% by weight, and the preferable upper limit is 50% by weight. When the content ratio of the segment derived from the polyfunctional (meth) acrylic monomer is less than 0.5% by weight, the effect of improving the thixotropy by the gel-like particles is hardly exhibited, and the obtained inorganic fine particle dispersed paste composition May be prone to stringing. When the content rate of the segment derived from the said polyfunctional (meth) acryl monomer exceeds 50 weight%, it will become insoluble in an organic solvent because a crosslinking degree becomes high too much, and the viscosity required for printing may not be obtained. The more preferable lower limit of the content ratio of the segment derived from the polyfunctional (meth) acrylic monomer is 1% by weight, and the more preferable upper limit is 40% by weight.

The gel particles preferably have a particle size of 10 μm or less. If the particle diameter exceeds 10 μm, it may cause voids in the sintered body or clogging during printing. A more preferable upper limit of the particle size of the gel-like particles is 5 μm, and a more preferable lower limit is 50 nm.
In this specification, “the particle size of the gel-like particles is 10 μm or less” means that 95% by weight or more of the gel-like particles pass through a filter having a pore size of 10 μm.

The preferable lower limit of the content of the gel particles in the inorganic fine particle dispersed paste composition of the present invention is 5% by weight, and the preferable upper limit is 20% by weight. When the content of the gel-like particles is less than 5% by weight, the resulting inorganic fine particle-dispersed paste composition may be inferior in moldability. When the content of the gel-like particles exceeds 20% by weight, the resulting inorganic fine particle-dispersed paste composition may be susceptible to stringing. A more preferable lower limit of the content of the gel-like particles is 7% by weight, and a more preferable upper limit is 15% by weight.

The gel-like particles containing the crosslinked (meth) acrylic resin are obtained by swelling resin fine particles containing a crosslinked (meth) acrylic resin with an organic solvent. By using such crosslinked resin fine particles, it is difficult to dissolve in an organic solvent and swells, so that stringing can be suppressed.
In the case of using uncrosslinked resin fine particles or core / shell fine particles having uncrosslinked sites instead of resin fine particles containing the above-mentioned crosslinked (meth) acrylic resin, a small amount is dissolved by dissolving a component having a high molecular weight in an organic solvent. This makes stringing easier to occur. In addition, the fine particles tend to aggregate and the viscosity is not stable.

The resin fine particles containing the crosslinked (meth) acrylic resin contain 70% by weight or more of the crosslinked (meth) acrylic resin. Thereby, melt | dissolution of resin fine particles can be suppressed and stringing can be suppressed. The crosslinked (meth) acrylic resin is preferably contained in an amount of 80% by weight or more.

The resin fine particles containing the crosslinked (meth) acrylic resin have a particle size of 10 μm or less. When the particle diameter of the resin fine particles containing the crosslinked (meth) acrylic resin is 10 μm or less, the inorganic fine particle-dispersed paste composition of the present invention has high viscosity and can reduce stringing, screen printing and dispensing. It can be suitably used for printing. On the other hand, when the particle diameter of the resin fine particles containing the crosslinked (meth) acrylic resin exceeds 10 μm, it causes voids in the sintered body, clogging during printing, and the like. The resin fine particles containing the crosslinked (meth) acrylic resin preferably have an upper limit of particle diameter of 5 μm.
Moreover, the minimum with a preferable particle diameter of the resin fine particle containing the said bridge | crosslinking (meth) acrylic resin is 10 nm. When the particle size is less than 10 nm, the compound is easily dissolved in an organic solvent, and the effect of improving thixotropy may be hardly exhibited.
A more preferable upper limit of the particle diameter of the resin fine particles containing the crosslinked (meth) acrylic resin is 5 μm, and a more preferable lower limit is 50 nm.
In this specification, “particle diameter of resin fine particles containing a crosslinked (meth) acrylic resin” is, for example, a dynamic light scattering particle size distribution meter (manufactured by Particle Sizing Systems, “NICOMP model 380 ZLS-S”). It was measured using.

The resin fine particles containing the crosslinked (meth) acrylic resin are preferably crosslinked solid fine particles, crosslinked hollow fine particles, or crosslinked core-shell fine particles.
The crosslinked solid fine particles are resin fine particles in which the entire particles are crosslinked.
The crosslinked hollow fine particles are resin fine particles in which the shell portion of the particles is crosslinked.
The crosslinked core-shell fine particles are resin fine particles in which both the core portion and the shell portion of the particles are crosslinked.

The gel-like particles can be produced by swelling resin fine particles containing a crosslinked (meth) acrylic resin with an organic solvent. In particular, when the resin fine particles containing the cross-linked (meth) acrylic resin are produced by suspension polymerization or emulsion polymerization, the cross-linked (meth) acrylic resin is obtained by centrifugation or freeze-drying. It is preferable that the resin fine particles are separated from an aqueous solution containing an ionic component, and the aqueous solution containing the ionic component is removed.

Since the gel-like particles are excellent in thickening, a sufficient viscosity can be secured in the resulting inorganic fine particle-dispersed paste composition. However, in the case where only the gel-like particles are too thixotropic and the viscosity becomes extremely low at the time of printing, the interaction of pseudo-crosslinking points can be suppressed by reducing the particle size of the gel-like particles, In addition to the gel particles, a thixotropic agent may be added as long as the purpose is not impaired.
The thixotropic agent is considered to be dispersed between the gel particles and reduce the thixotropy by reducing the interaction between the gel particles.
Examples of the thixotropy reducing agent include other binder resins, resins having low stringiness such as liquid polymers, and crystalline organic compounds such as crystalline polyhydric alcohol-based organic compounds having excellent viscosity increase due to hydrogen bonding. .

The binder resin used as the thixotropic agent is not particularly limited, and examples thereof include cellulose resin, (meth) acrylic resin, polyether resin, polyacetal resin, polyvinyl acetal resin, and rosin resin. Among them, polyether resin, (meth) acrylic resin, and rosin resin can be suitably used because of high thermal decomposability and low residual carbon after sintering.

Although it does not specifically limit as a liquid polymer used as said thixotropic property reducing agent, For example, a low molecular weight acrylic oligomer and polyether resin can be used suitably.
The crystalline polyhydric alcohol-based organic compound used as the thixotropic agent is not particularly limited, and examples thereof include 2,2-dimethyl-1,3-propanediol and 2,2-diethyl-1,3-propane. Diol, 2-butyl-2-ethyl-1,3-propanediol, trimethylolethane, trimethylolpropane and the like can be suitably used.

The minimum with preferable content of the said thixotropy reducing agent in the inorganic fine particle dispersion paste composition of this invention is 0.2 weight%, and a preferable upper limit is 25 weight%. If the content of the thixotropic agent is less than 0.2% by weight, the effect of reducing the thixotropic property may not be obtained. When the content of the thixotropy reducing agent exceeds 25% by weight, the resulting inorganic fine particle-dispersed paste composition may be susceptible to stringing. The more preferable lower limit of the thixotropic agent is 0.5% by weight, and the more preferable upper limit is 20% by weight.

The inorganic fine particle-dispersed paste composition of the present invention contains inorganic fine particles.
The inorganic fine particles are not particularly limited, but those using at least one selected from the group consisting of metals, glasses, silicon compounds, carbon black, tin-containing alloys, and metal complexes as raw materials are preferably used.
Specifically, for example, copper, silver, platinum, gold, silver, aluminum, tungsten, nickel, palladium, alumina, zirconia, titanium oxide, magnesium oxide, ITO, barium titanate, alumina nitride, silicon nitride, boron nitride, silica glasses, low melting point such as lead _{glass, CaO · Al 2 O 3 ·} SiO 2 type inorganic _{glass, MgO · Al 2 O 3 ·} SiO 2 type inorganic _{glass, LiO 2 · Al 2 O 3} · SiO 2 type inorganic glass Glass, bismuth oxide glass, silicate glass, lead glass, zinc glass, boron glass, silicon compound, various carbon blacks, solder powder, metal complex, blue phosphor material conventionally known as inorganic phosphor material, red A phosphor material, a green phosphor material, or the like is used. Examples of the blue phosphor material include Y ₂ SiO ₅ : Ce, CaWO ₄ : Pb, BaMgAl ₁₀ O ₁₇ : Eu, BaMgAl ₁₄ O ₂₃ : Eu, BaMgAl ₁₆ O ₂₇ : Eu, and BaMg ₂ Al. ₁₄ O ₂₃ : Eu, BaMg ₂ Al ₁₄ O ₂₇ : Eu, and ZnS: (Ag, Cd) are used. Examples of the red phosphor material include Y ₂ O ₃ : Eu, Y ₂ SiO ₅ : Eu, Y ₃ Al ₅ O ₁₂ : Eu, Zn ₃ (PO ₄ ) ₂ : Mn, YBO ₃ : Eu. System, (Y, Gd) BO ₃ : Eu system, GdBO ₃ : Eu system, ScBO ₃ : Eu system, and LuBO ₃ : Eu system are used. Examples of the green phosphor material include Zn ₂ SiO ₄ : Mn, BaAl ₁₂ O ₁₉ : Mn, SrAl ₁₃ O ₁₉ : Mn, CaAl ₁₂ O ₁₉ : Mn, YBO ₃ : Tb, BaMgAl ₁₄ O ₂₃ : Mn-based, LuBO ₃ : Tb-based, GdBO ₃ : Tb-based, ScBO ₃ : Tb-based, Sr6Si ₃ O ₃ Cl ₄ : Eu-based are used. In addition, ZnO: Zn system, ZnS: (Cu, Al) system, ZnS: Ag system, Y ₂ O ₂ S: Eu system, ZnS: Zn system, (Y, Cd) BO ₃ : Eu system, BaMgAl ₁₂ O ₂₃ : Eu type can also be used. Etc.

The content of the inorganic fine particles is not particularly limited, but in the inorganic fine particle-dispersed paste composition of the present invention, it is added to 100 parts by weight of a binder resin composition composed of components other than the inorganic fine particles such as the gel particles and the organic solvent described later. On the other hand, a preferred lower limit is 10 parts by weight and a preferred upper limit is 300 parts by weight. If the content of the inorganic fine particles is less than 10 parts by weight, sufficient thixotropy may not be obtained in the inorganic fine particle dispersed paste composition. When the content of the inorganic fine particles exceeds 300 parts by weight, it may be difficult to disperse the inorganic fine particles.

In addition, the inorganic fine particle dispersed paste composition of the present invention preferably contains a nonionic surfactant having an HLB value of 10 or more in order to appropriately stabilize the dispersion state of the inorganic fine particles. Here, the HLB value is used as an index representing the hydrophilicity and lipophilicity of a surfactant, and several calculation methods have been proposed. For example, for a nonionic surfactant, the saponification value is S When the acid value of the fatty acid constituting the surfactant is A, the HLB value is defined as 20 (1-S / A).
The nonionic surfactant having an HLB value of 10 or more is not particularly limited, but those obtained by adding an alkylene ether to the fatty chain are preferred. Specific examples include polyoxyethylene lauryl ether and polyoxyethylene cetyl ether. Etc. are suitable. The nonionic surfactant has good thermal decomposability, but if added in a large amount, the thermal decomposability of the inorganic fine particle-dispersed paste composition may be lowered. Therefore, the preferable upper limit of the content is 5% by weight. .

The inorganic fine particle dispersed paste composition of the present invention contains an organic solvent. Although the said organic solvent will not be specifically limited if it is a solvent which swells particle | grains, The organic solvent whose boiling point is 160 degreeC or more and less than 290 degreeC is suitable. If the boiling point of the organic solvent is less than 160 ° C, the paste may dry during printing. If the boiling point of the organic solvent is 290 ° C. or higher, enormous energy is required for drying.
The organic solvent having a boiling point of 160 ° C. or higher and lower than 290 ° C. is not particularly limited.
Ethylene glycol monomethyl ether, ethylene glycol ethyl ether, ethylene glycol monobutyl ether, ethylene glycol dodecyl ether, ethylene glycol monomethyl ether acetate, ethylene glycol ethyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol dodecyl ether acetate, ethylene glycol dimethyl ether, ethylene glycol Diethyl ether, ethylene glycol dibutyl ether, ethylene glycol ethyl methyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol mono nbutyl ether, diethylene glycol monoisobutyl ether, diethylene glycol Nohexyl ether, diethylene glycol monooleate, diethylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetate, diethylene glycol mono nbutyl ether acetate, diethylene glycol monoisobutyl ether acetate, diethylene glycol monohexyl ether acetate, diethylene glycol monooleate acetate, diethylene glycol monophenyl ether acetate, Diethylene glycol monolaurate, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol di-n-butyl ether, triethylene glycol diacetate, triethylene glycol dimethyl ether, triethylene glycol Monobutyl ether, triethylene glycol monostearate, triethylene glycol monobenzyl ether, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, propylene glycol diacetate, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monopropyl ether , Dipropylene glycol monobutyl ether, dipropylene glycol monomethyl ether acetate, dipropylene glycol monopropyl ether acetate, dipropylene glycol monobutyl ether acetate, tripropylene glycol monomethyl ether, tripropylene glycol monomethyl ether acetate tetraethylene glycol, tetra Ethylene glycol dodecyl ether, tetraethylene glycol monooctyl ether, tetraethylene glycol monomethyl ether, pentaethylene glycol dodecyl ether, heptaethylene glycol dodecyl ether, hexaethylene glycol dodecyl ether, diethylene glycol monophenyl ether, ethylene glycol monobenzyl ether, diethylene glycol monobenzyl ether Ether, propylene glycol monophenyl ether, terpineol, texanol, butyl carbitol, butyl carbitol acetate, isophorone, butyl lactate, dioctyl phthalate, dioctyl adipate, benzyl alcohol, phenyl propylene glycol, cresol, phenyl glycol, terpineol acetate , Dihydroterpineol, dihydroterpineol acetate, 1,3-butanediol, 1,5-pentanediol, 3-methoxy-3-methyl-1-butanol, 3-methyl-1,3-butanediol, 3-methyl -1,5-pentanediol, 2,4-diethyl-1,5-pentanediol, 2-ethyl-1,3-hexanediol and the like. Among these, terpineol, butyl carbitol, butyl carbitol acetate, texanol, benzyl alcohol, phenyl glycol, 2-ethyl-1,3-hexanediol, 3-methyl-1,3-butanediol and the like are preferably used. These organic solvents may be used independently and 2 or more types may be used together.

The inorganic fine particle-dispersed paste composition of the present invention preferably has as little impurity ion content as possible, and the preferable upper limit of the impurity ion concentration is 0.5 ppm. When the concentration of the impurity ions exceeds 0.5 ppm, it becomes difficult to use the obtained inorganic fine particle dispersed paste composition for semiconductor-related applications. The density | concentration of the said impurity ion can be 0.5 ppm or less by manufacturing the said gel-like particle | grains with the method mentioned above.

Specific examples of the impurity ions include alkali metal ions, and more specifically, sodium ions.
Examples of the method for measuring the concentration of impurity ions include a method for evaluating from the relationship between a potential difference such as a potential difference analysis method and an electrolytic current, an emission spectroscopy method, a high-frequency inductively coupled plasma (ICP emission analysis method), and the like.

In addition, the inorganic fine particle-dispersed paste composition of the present invention has a viscosity of 10 Pa · s or more and less than 100 Pa · s when measured with a B-type viscometer at 23 ° C. and setting the probe rotation speed to 10 rpm. preferable. When the viscosity is less than 10 Pa · s, it may be naturally cast when it is left standing and dried after printing by screen printing or the like. When the viscosity is 100 Pa · s or more, the resulting inorganic fine particle-dispersed paste composition may have printability.

The inorganic fine particle dispersed paste composition of the present invention preferably has a TI value (thixotropic property) represented by the following formula (1) of 1.0 to 3.0. When the TI value exceeds 3.0, a sudden change in viscosity may occur due to shear that the inorganic fine particle dispersed paste composition undergoes during printing. In addition, when used for screen printing, the inorganic fine particle dispersed paste composition may scatter and a printed image may not be formed. Furthermore, when used for dispensing printing, the paste may not be discharged straight from the nozzle due to the inorganic fine particle dispersed paste composition being discharged at a stroke. A more preferable upper limit of the TI value is 2.5.

  TI value = (viscosity at 10 rpm) / (viscosity at 100 rpm) (1)

The method for producing the inorganic fine particle-dispersed paste composition of the present invention is not particularly limited, and the above-mentioned gel-like particles, inorganic fine particles, organic solvent, and the like, and a thixotropy reducing agent are conventionally known stirring using a three roll or the like. The method of stirring by a method is mentioned.

Although the use of the inorganic fine particle dispersion paste composition of the present invention is not particularly limited, it can be suitably used for LED backlights, plasma display panels, VDF panels, inorganic EL, solar cell panels and the like.

According to the present invention, it is possible to provide an inorganic fine particle-dispersed paste composition that has a high viscosity, is excellent in screen printability and dispense printability, and can be fired at a low temperature.

Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.
Example 1
(Preparation of slurry containing gel particles)
As a monomer component, 15 parts by weight of polytetramethylene glycol dimethacrylate (the number of polytetramethylene glycol units = about 1; manufactured by Hitachi Chemical Co., Ltd., FA-124M), and 100 parts by weight of a monomer mixed with 85 parts by weight of ethyl methacrylate, In addition to 100 weight part of 0.5 weight% aqueous solution of anionic surfactant Haitenol LA-12 (Daiichi Kogyo Seiyaku Co., Ltd.), the mixture was stirred using a stirring and dispersing device to obtain an emulsified suspension.
Next, using a 2 liter polymerization vessel equipped with a stirrer, jacket, reflux condenser and thermometer, the inside of the polymerization vessel was depressurized, the vessel was deoxygenated, and then the pressure was returned to atmospheric pressure with nitrogen gas. The inside of the polymerization vessel was set to a nitrogen atmosphere. In this polymerization vessel, 200 parts by weight of water was added, and after the temperature of the polymerization vessel was raised to 70 ° C., 0.5 parts by weight of ammonium persulfate as a polymerization initiator and 5 parts by weight of the above emulsion suspension were seed monomers. To start polymerization. After aging for 30 minutes, the remaining emulsified suspension was added dropwise over 2 hours. After further aging for 2 hours, the polymerization vessel was cooled to room temperature to obtain a slurry of resin fine particles (a). It was 152 nm when the particle diameter of the obtained resin fine particles (a) was measured. The particle diameter (volume average particle diameter) of the resin fine particles (a) was measured by using a dynamic light scattering type particle size distribution meter (manufactured by Particle Sizing Systems, “NICOMP model 380 ZLS-S”).
The solvent of the obtained resin fine particle (a) slurry was replaced with terpineol by using a centrifuge to obtain a terpineol dispersion of gel-like particles (A).

(Preparation of inorganic fine particle dispersed paste composition)
40.5 parts by weight of terpineol, 0.5 part by weight of BL25 (manufactured by Nikko Chemicals) as a nonionic surfactant, 7 parts by weight of polyether polyol (manufactured by Asahi Glass Co., Ltd., Preminol 4015), phosphor powder (manufactured by Nichia Corporation) , Zn ₂ SiO ₄ : Mn), 40 parts by weight of gel particles (A) were added so as to have the composition shown in Table 2, and mixed uniformly using a three roll mill to obtain an inorganic fine particle dispersed paste composition. It was.

(Example 2)
(Preparation of slurry containing gel particles)
The solvent of the resin fine particle (b) slurry obtained in the same manner as in Example 1 except that 10 parts by weight of polytetramethylene glycol dimethacrylate and 90 parts by weight of butyl methacrylate were blended as a monomer component was centrifuged. Was replaced with terpineol to obtain a terpineol dispersion of gel particles (B).

(Preparation of inorganic fine particle dispersed paste composition)
Add 42.5 parts by weight of terpineol, 0.5 parts by weight of BL25 (manufactured by Nikko Chemicals) as a nonionic surfactant, and 40 parts by weight of solder powder particles (manufactured by Nippon Solder Co., Ltd., “VO”, average particle diameter 2 μm). Then, a bead mill treatment was performed for 1 hour using a bead mill (manufactured by Imex Corporation, “RMB-08”) and zirconia particles having a particle diameter of 1 mm as a medium to obtain a slurry.
Next, gel particles (B) and 7 parts by weight of polyether polyol are added to the resulting slurry so as to have the composition shown in Table 2, and mixed uniformly using a three-roll mill, and an inorganic fine particle dispersed paste composition Got.

(Example 3)
(Preparation of inorganic fine particle dispersed paste composition)
53.5 parts by weight of terpineol is blended, and 30 parts by weight of silver fine particles (manufactured by Metallow, average particle size 1 μm) are blended instead of 40 parts by weight of phosphor powder (manufactured by Nichia Corporation, Zn ₂ SiO ₄ : Mn). An inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 1 except that the gel particles (B) were added so as to have the composition shown in Table 2.

Example 4
(Preparation of inorganic fine particle dispersed paste composition)
51.5 parts by weight of terpineol was blended, and instead of 40 parts by weight of phosphor powder (manufactured by Nichia Chemical Co., Ltd., Zn ₂ SiO ₄ : Mn), glass fine particles having an average particle diameter of 2.0 μm (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) 30 parts by weight was blended, and an inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 1 except that the gel particles (B) were added so as to have the blends shown in Table 2.

(Example 5)
(Preparation of inorganic fine particle dispersed paste composition)
41.5 parts by weight of terpineol is blended, and phosphor powder (manufactured by Nichia Corporation, (Y, Gd) BO ₃ is used instead of 40 parts by weight of phosphor powder (manufactured by Nichia Corporation, Zn ₂ SiO ₄ : Mn)). : Eu) An inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 1 except that 40 parts by weight was blended and the gel-like particles (B) were added so as to be blended as shown in Table 2.

(Example 6)
(Preparation of inorganic fine particle dispersed paste composition)
Instead of terpineol, 41.5 parts by weight of texanol is blended, and phosphor powder (manufactured by Nichia Corporation, BaMgAl ₁₀ ) instead of 40 parts by weight of phosphor powder (manufactured by Nichia Chemical Co., Ltd., Zn ₂ SiO ₄ : Mn). Inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 1 except that 40 parts by weight of O ₁₇ : Eu) was added and the gel particles (B) were added so as to have the composition shown in Table 2. .

(Example 7)
(Preparation of slurry containing gel particles)
The solvent of the resin fine particle (c) slurry obtained in the same manner as in Example 1 except that 15 parts by weight of polytetramethylene glycol dimethacrylate and 85 parts by weight of butyl methacrylate were blended as a monomer component was centrifuged. Was replaced with terpineol to obtain a terpineol dispersion of gel particles (C).

(Preparation of inorganic fine particle dispersed paste composition)
40.5 parts by weight of terpineol, 7 parts by weight of polyether polyol (Asahi Glass Co., Ltd., Preminol 4015), and gel particles (C) added in place of the gel particles (B) so as to have the composition shown in Table 2. Except for the above, an inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 5.

(Example 8)
(Preparation of slurry containing gel particles)
Obtained in the same manner as in Example 1 except that 15 parts by weight of polytetramethylene glycol dimethacrylate, 75 parts by weight of butyl methacrylate, and 10 parts by weight of stearyl methacrylate (Blenmer SMA) were blended as monomer components. The solvent of the obtained resin fine particle (d) slurry was replaced with terpineol by using a centrifuge to obtain a terpineol dispersion of gel-like particles (D).

(Preparation of inorganic fine particle dispersed paste composition)
An inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 7 except that the gel particles (D) were added instead of the gel particles (C) so as to have the formulation shown in Table 2.

Example 9
(Preparation of slurry containing gel particles)
As in Example 1, except that 15 parts by weight of polytetramethylene glycol dimethacrylate, 75 parts by weight of butyl methacrylate, and 10 parts by weight of polypropylene glycol monomethacrylate (manufactured by NOF Corporation, Blenmer PP1000) were blended as monomer components. The solvent of the resin fine particle (e) slurry obtained in this way was replaced with terpineol using a centrifuge to obtain a terpineol dispersion of gel-like particles (E).

(Preparation of inorganic fine particle dispersed paste composition)
An inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 7 except that gel particles (E) were added instead of the gel particles (C) so as to have the composition shown in Table 2.

(Example 10)
(Preparation of slurry containing gel particles)
The same as in Example 1 except that 15 parts by weight of polytetramethylene glycol dimethacrylate, 75 parts by weight of butyl methacrylate, and 10 parts by weight of methoxypolyethylene glycol monomethacrylate (manufactured by NOF Corporation, Blemmer PME1000) were blended as monomer components. The solvent of the resin fine particle (f) slurry obtained in this manner was replaced with terpineol using a centrifuge, thereby obtaining a terpineol dispersion of gel-like particles (F).

(Preparation of inorganic fine particle dispersed paste composition)
An inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 7 except that the gel-like particles (F) were added instead of the gel-like particles (C) so as to have the formulation shown in Table 2.

(Example 11)
(Preparation of inorganic fine particle dispersed paste composition)
Except that 38.5 parts by weight of terpineol, 7 parts by weight of polyether polyol (manufactured by Asahi Glass Co., Ltd., Preminol 4015) and 2 parts by weight of trimethylolpropane were added so as to have the composition shown in Table 2, the same manner as in Example 7 was performed. Thus, an inorganic fine particle dispersed paste composition was obtained.

(Example 12)
(Preparation of inorganic fine particle dispersed paste composition)
Example 7 except that 35.5 parts by weight of terpineol and 5 parts by weight of 2-butyl-2-ethyl-1,3-propanediol instead of trimethylolpropane were added so as to have the composition shown in Table 2. In the same manner, an inorganic fine particle dispersed paste composition was obtained.

(Example 13)
(Preparation of inorganic fine particle dispersed paste composition)
An inorganic fine particle-dispersed paste composition was obtained in the same manner as in Example 7 except that preminol 3011 was added in place of preminol 4015 so as to have the composition shown in Table 2.

(Example 14)
(Preparation of inorganic fine particle dispersed paste composition)
Inorganic fine particles in the same manner as in Example 12, except that 34.5 parts by weight of terpineol and 13 parts by weight of gel-like particles (A) instead of gel-like particles (C) were added so as to have the composition shown in Table 2. A dispersion paste composition was obtained.

(Comparative Example 1)
(Preparation of inorganic fine particle dispersed paste composition)
Example 5 was repeated except that 32.5 parts by weight of terpineol, 12 parts by weight of trimethylolpropane, and 15 parts by weight of polyether polyol were added so as to have the composition shown in Table 2 without adding the resin fine particles. An inorganic fine particle dispersed paste composition was obtained.
The obtained inorganic fine particle-dispersed paste composition had a high viscosity and was stringed, so that screen printing and dispense printing could not be performed. In the storage stability evaluation, phase separation occurred.

(Comparative Example 2)
(Preparation of slurry containing gel particles)
As a particle core part, a total amount of 100 parts by weight of a monomer obtained by mixing 15 parts by weight of polytetramethylene glycol dimethacrylate (the number of polytetramethylene glycol units = about 1; manufactured by Hitachi Chemical Co., Ltd., FA-124M) and 85 parts by weight of butyl methacrylate. , Anionic surfactant Hytenol LA-12 (Daiichi Kogyo Seiyaku Co., Ltd.) 0.5 wt% aqueous solution 100 parts by weight and stirred using a stirring and dispersing device to obtain an emulsified suspension of the core part .
As a particle shell part, 100 parts by weight of a monomer mixed with 100 parts by weight of butyl methacrylate was added to 100 parts by weight of a 0.5% by weight aqueous solution of anionic surfactant Hitenol LA-12 (Daiichi Kogyo Seiyaku Co., Ltd.). The mixture was stirred using a stirring and dispersing device to obtain an emulsified suspension in the shell portion.
Next, using a 2 liter polymerization vessel equipped with a stirrer, jacket, reflux condenser and thermometer, the inside of the polymerization vessel was depressurized, the vessel was deoxygenated, and then the pressure was returned to atmospheric pressure with nitrogen gas. The inside of the polymerization vessel was set to a nitrogen atmosphere. In this polymerization vessel, 200 parts by weight of water was added, and after the temperature of the polymerization vessel was raised to 70 ° C., 0.5 part by weight of ammonium persulfate as a polymerization initiator and the emulsification suspension of the core part among the above emulsion suspensions Polymerization was started by adding 5 parts by weight of the liquid as a seed monomer. After aging for 30 minutes, 95 parts by weight of the emulsion suspension in the shell part was added dropwise over 2 hours. After further aging for 2 hours, the polymerization vessel was cooled to room temperature to obtain a slurry of resin fine particles (g). It was 175 nm when the particle diameter of the obtained resin fine particles (g) was measured. The particle size (volume average particle size) of the resin fine particles (g) was measured by using a dynamic light scattering particle size distribution meter (“NICOMP model 380 ZLS-S”, manufactured by Particle Sizing Systems).
The resin fine particles (g) are core-shell particles whose core is a crosslinked (meth) acrylic resin and whose shell is an uncrosslinked (meth) acrylic resin, and the content of the crosslinked (meth) acrylic resin is 50% by weight. It was.
The solvent of the obtained resin fine particle (g) slurry was replaced with terpineol using a centrifugal separator to obtain a terpineol dispersion of gel-like particles (G).

(Preparation of inorganic fine particle dispersed paste composition)
Inorganic fine particles in the same manner as in Example 5 except that 40.5 parts by weight of terpineol and 12 parts by weight of gel-like particles (G) instead of gel-like particles (B) were added so as to have the composition shown in Table 2. A dispersion paste composition was obtained.
The obtained inorganic fine particle-dispersed paste composition had a low viscosity, but was strong in stringing and could not be printed by both screen printing and dispensing printing. This is thought to be because fine particles not cross-linked were dissolved.

(Comparative Example 3)
(Preparation of slurry containing gel particles)
As a particle core part, 15 parts by weight of polytetramethylene glycol dimethacrylate (number of polytetramethylene glycol units = about 1; manufactured by Hitachi Chemical Co., Ltd., FA-124M), 85 parts by weight of butyl methacrylate, and azobisiso as a polymerization initiator A monomer solution was prepared by mixing and stirring 0.3 parts by weight of butyronitrile (AIBN).
The total amount of the monomer solution thus obtained is added to 300 parts by weight of an aqueous solution of 1% by weight polyvinyl alcohol (PVA) and 0.02% by weight sodium nitrite, and stirred using a stirring and dispersing device to obtain an emulsified suspension. It was.
Next, using a 2 liter polymerization vessel equipped with a stirrer, jacket, reflux condenser and thermometer, the inside of the polymerization vessel was depressurized, the vessel was deoxygenated, and then the pressure was returned to atmospheric pressure with nitrogen gas. The inside of the polymerization vessel was set to a nitrogen atmosphere. The entire amount of the emulsified suspension obtained above was charged all at once into this polymerization vessel, and the polymerization vessel was heated to 60 ° C. to initiate polymerization. After polymerization for 8 hours, the polymerization vessel was cooled to room temperature to obtain a slurry of resin fine particles (h). When the particle diameter of the obtained resin fine particles (h) was measured and the solvent of the obtained resin fine particle (h) slurry, which was 54 μm, was replaced with terpineol using a centrifuge, gel particles (H A terpineol dispersion was obtained.

(Preparation of inorganic fine particle dispersed paste composition)
Inorganic fine particles in the same manner as in Example 5, except that 40.5 parts by weight of terpineol and 12 parts by weight of gel-like particles (H) instead of the gel-like particles (B) were added so as to have the composition shown in Table 2. A dispersion paste composition was obtained.
The obtained inorganic fine particle-dispersed paste composition could not be printed due to clogging in both screen printing and dispensing printing.

(Comparative Example 4)
(Preparation of slurry containing gel particles)
As a monomer component, 100 parts by weight of a monomer mixed with 100 parts by weight of butyl methacrylate was added to 100 parts by weight of an anionic surfactant Hytenol LA-12 (Daiichi Kogyo Seiyaku Co., Ltd.) 0.5% by weight aqueous solution, The mixture was stirred using a stirring and dispersing device to obtain an emulsified suspension.
Next, using a 2 liter polymerization vessel equipped with a stirrer, jacket, reflux condenser and thermometer, the inside of the polymerization vessel was depressurized, the vessel was deoxygenated, and then the pressure was returned to atmospheric pressure with nitrogen gas. The inside of the polymerization vessel was set to a nitrogen atmosphere. In this polymerization vessel, 200 parts by weight of water was added, and after the temperature of the polymerization vessel was raised to 70 ° C., 0.5 parts by weight of ammonium persulfate as a polymerization initiator and 5 parts by weight of the above emulsion suspension were seed monomers. To start polymerization. After aging for 30 minutes, the remaining emulsified suspension was added dropwise over 2 hours. After further aging for 2 hours, the polymerization vessel was cooled to room temperature to obtain a slurry of resin fine particles (i). The particle diameter of the obtained resin fine particles (i) was measured and found to be 135 nm.
The solvent of the obtained resin fine particle (i) slurry was replaced with terpineol using a centrifuge, thereby obtaining a terpineol dispersion of gel-like particles (I).

(Preparation of inorganic fine particle dispersed paste composition)
Inorganic fine particles in the same manner as in Example 5 except that 40.5 parts by weight of terpineol and 12 parts by weight of gel-like particles (I) instead of gel-like particles (B) were added so as to have the composition shown in Table 2. A dispersion paste composition was obtained.
The obtained inorganic fine particle-dispersed paste composition was strongly stringed because the particles were dissolved in a solvent, and could not be printed by both screen printing and dispensing printing.

<Evaluation>
The following (1) to (9) were evaluated for the inorganic fine particle dispersed paste compositions obtained in Examples 1 to 14 and Comparative Examples 1 to 4. The results are shown in Table 2.
Table 1 shows the composition and particle diameter (volume average particle diameter) of the resin fine particles (a) to (i).
In addition, the particle diameter measured the volume average particle diameter by using the dynamic light-scattering type particle size distribution analyzer (Participating Systems company make, "NICOMP model 380 ZLS-S").

(1) Filtration 100 g of the inorganic fine particle-dispersed paste composition obtained in Examples and Comparative Examples was filtered using a cartridge filter (PMC-100, manufactured by Nippon Filter Co., Ltd.) having a pore size of 10 μm. The case where the particle component completely passed through the filter was evaluated as “◯”, and the case where there was a particle component that could not pass through the filter was evaluated as “x”.

(2) Viscosity Viscosity of the inorganic fine particle-dispersed paste compositions obtained in the examples and comparative examples was measured using a B-type viscometer (“DVII + Pro” manufactured by BROOK FILED) at a probe rotation speed of 10 rpm at 23 ° C. Evaluated. When the viscosity was 10 Pa · s or more, it was judged that the thickening ability was high.

(3) TI value Using the B-type viscometer ("DVII + Pro", manufactured by BROOK FILED), the inorganic fine particle dispersed paste composition obtained in the examples and comparative examples was used at 23 ° C, at a probe rotation speed of 10, 100 rpm. Viscosity was measured at, and the TI value was calculated from the following formula (1). When the TI value was in the range of 1.0 to 3.0, it was determined that the print adaptability was excellent.

TI value = (viscosity at 10 rpm) / (viscosity at 100 rpm) (1)

(4) Containing ion analysis The inorganic fine particle dispersed paste compositions obtained in the Examples and Comparative Examples were subjected to a high frequency output of 1.2 kW and a plasma gas flow rate of 15 L using an ICP emission analyzer (“SPS5000” manufactured by Seiko). The amount of Na ions was measured under the conditions of / min and a carrier gas flow rate of 0.75 L / min.

(5) A stainless steel pick with a diameter of 2.6 mm with a sharpened tip is inserted into the inorganic fine particle dispersed paste composition obtained in Examples and Comparative Examples to a depth of 10 mm and pulled vertically at a constant speed of 500 mm / min. It was. After the inorganic fine particle-dispersed paste composition attached to the stainless steel pick was stretched and the yarn was broken, the pick was stopped from rising, and the length of the paste composition was stabilized. The stainless pick was laid at 90 degrees, and the length of stringing from the tip of the stainless pick was evaluated. When the stringing length is 10 mm or less, it can be said that the printability is excellent.

(6) Screen printing property The obtained inorganic fine particle dispersed paste composition was applied to a screen printing machine ("MT-320TV" manufactured by Microtech Co., Ltd.), screen plate making ("SX320" manufactured by Tokyo Process Service Co., Ltd.), emulsion 20 [mu], printed image 80 mm. Printing was performed in an environment of a temperature of 23 ° C. and a humidity of 50% using a solid of 80 mm, a screen frame: 320 mm × 320 mm, and a printed glass substrate (soda glass: 150 mm × 150 mm, thickness: 1.5 mm).
After printing, the solvent was dried in a blast oven on the glass plate at 120 ° C. for 10 minutes.
Further, 30 sheets were continuously printed, and the image blurring state was confirmed.
The case where no change was observed by continuous printing of 30 sheets was evaluated as “◯”, and the case where blurring occurred due to clogging was evaluated as “X”.

(7) Dispense printability Dispense printing machine (Musashi Engineering Co., Ltd., “SHOTMASTER300”), Dispensing nozzle (Musashi Engineering Co., Ltd., “NH-015N”), glass separated from the nozzle by 5 cm with a discharge pressure of 0.5 MPa. The operation of dispensing the inorganic fine particle-dispersed paste compositions obtained in Examples and Comparative Examples on the plate was performed 10 times, and the clogged state of the nozzles was evaluated. The case where clogging did not occur was evaluated as “◯”, and the case where clogging occurred was evaluated as “x”.

(8) Dispense printability (paste behavior immediately after discharge)
Dispense printing machine (Musashi Engineering Co., Ltd., “SHOTMASTER 300”), Dispensing nozzle (Musashi Engineering Co., Ltd., “NH-015N”), on a glass plate 5 cm away from the nozzle with a discharge pressure of 0.5 MPa. The operation of dispensing printing the inorganic fine particle dispersed paste composition obtained in the comparative example was performed 10 times, and it was evaluated whether or not the discharged paste reached the glass substrate straight from the nozzle. The case where the paste reached the glass substrate straight was evaluated as “◯”, and the case where the paste adhered to the nozzle or did not reach the glass substrate was evaluated as “x”.

(9) Storage stability After the inorganic fine particle-dispersed paste composition obtained in the Examples and Comparative Examples was allowed to stand in a thermostatic chamber at 23 ° C. for 2 weeks, the state of the paste was confirmed by visual observation, and the layer separation was also performed using inorganic fine particles. The case where no sedimentation was observed was evaluated as “◯”, and the case where it was separated into two layers and the inorganic fine particles were sedimented was evaluated as “x”.

According to the present invention, it is possible to provide an inorganic fine particle-dispersed paste composition that has a high viscosity, is excellent in screen printability and dispense printability, and can be fired at a low temperature.

Claims (9)

An inorganic fine particle-dispersed paste composition containing gel-like particles containing a crosslinked (meth) acrylic resin, inorganic fine particles and an organic solvent,
The gel-like particles containing the crosslinked (meth) acrylic resin are obtained by swelling resin fine particles containing 70% by weight or more of a crosslinked (meth) acrylic resin with the organic solvent,
The particle diameter of resin fine particles containing 70% by weight or more of the crosslinked (meth) acrylic resin is 10 μm or less, and
The cross-linked (meth) acrylic resin is a copolymer having a segment derived from a monofunctional (meth) acrylic monomer and a segment derived from a polyfunctional (meth) acrylic monomer. object. The inorganic fine particle-dispersed paste composition according to claim 1, wherein the cross-linked (meth) acrylic resin has a content ratio of a segment derived from a polyfunctional (meth) acrylic monomer of 0.5 to 50% by weight. The inorganic fine particle-dispersed paste composition according to claim 1 or 2, wherein the organic solvent has a boiling point of 160 ° C or higher and lower than 290 ° C. 4. The viscosity according to claim 1, wherein the viscosity is 10 Pa · s or more and less than 100 Pa · s when measured with a B-type viscometer at 23 ° C. with the probe rotation speed set to 10 rpm. Inorganic fine particle dispersed paste composition. An LED backlight comprising the inorganic fine particle dispersed paste composition according to claim 1, 2, 3 or 4. 5. A plasma display panel using the inorganic fine particle dispersed paste composition according to claim 1, 2, 3 or 4. A VDF panel comprising the inorganic fine particle dispersed paste composition according to claim 1, 2, 3 or 4. An inorganic EL comprising the inorganic fine particle dispersed paste composition according to claim 1, 2, 3 or 4. A solar cell panel comprising the inorganic fine particle dispersed paste composition according to claim 1, 2, 3 or 4.