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WO2002018080A1 - Composition de solution colloidale metallique et conducteur ou encre destine a la formation d'un motif semi-conducteur la renfermant, et procede de formation d'un motif conducteur ou semi-conducteur - Google Patents

Composition de solution colloidale metallique et conducteur ou encre destine a la formation d'un motif semi-conducteur la renfermant, et procede de formation d'un motif conducteur ou semi-conducteur Download PDF

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Publication number
WO2002018080A1
WO2002018080A1 PCT/JP2001/006655 JP0106655W WO0218080A1 WO 2002018080 A1 WO2002018080 A1 WO 2002018080A1 JP 0106655 W JP0106655 W JP 0106655W WO 0218080 A1 WO0218080 A1 WO 0218080A1
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Prior art keywords
group
metal
conductor
forming
solution composition
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English (en)
Japanese (ja)
Inventor
Kazunori Kataoka
Yukio Nagasaki
Takeshi Sakura
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Upepo and Maji Inc
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Upepo and Maji Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
    • H05K3/105—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by conversion of non-conductive material on or in the support into conductive material, e.g. by using an energy beam
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
    • H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
    • H05K3/1241—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by ink-jet printing or drawing by dispensing

Definitions

  • the present invention relates to a metal colloid solution composition, an ink for forming a conductor or semiconductor pattern using the same, and a method for forming a conductor or semiconductor pattern.
  • the present invention relates to a metal colloid solution composition and a method for producing an industrial material using the composition. More specifically, a highly dispersed metal or metal oxide colloid solution composition that can be used as a catalyst, an electric material, a magnetic material, an optical material, and the like; The present invention relates to a method for forming a non-conductive substrate. Background art
  • Colloids are fine particles with a size of 1 to 500 nm, and are generally defined as a dispersion uniformly dispersed in a solvent.
  • metal colloids have been actively studied for application as functional materials.
  • Metal colloids unlike bulk metals, have a very large specific surface area and therefore exhibit unique behavior different from ordinary metal atoms. Utilization of such properties of metal colloids is expected to be applied to catalysts, electric materials, magnetic materials, optical materials, sensors, and so on.
  • metal colloid solutions using a water-soluble polymer or a surfactant as a protective agent generally have poor storage stability.
  • the protective agent undergoes dehydration and coagulates, and is therefore unstable.
  • surfactants or polymer compounds are used as protective agents for stabilizing metal colloid solutions. Such a protective agent physically or chemically bonds to the surface of the metal particles and attempts to stabilize the dispersion by sterically repelling the particles.
  • polymers are more effective as protective agents than surfactants, and proteins such as gelatin and albumin and water-soluble polymers such as polyvinyl alcohol and polybierpyrrolidone are used.
  • a method for preparing a metal colloid solution is disclosed, for example, in JP-A-8-27307.
  • all of these disclosed prior art colloid solutions have only a hydrophilic polymer or a hydrophobic polymer bound to the metal surface. For this reason, the solvent is very limited.
  • ordinary polymers have poor physical or chemical adsorptivity of terminal functional groups to metals or metal oxides and poor storage stability.
  • a metal foil is first provided on the entire surface of a substrate, and a photo-curable resin is masked with a photoresist ink on a desired portion, and then immersed in a solution for dissolving the metal. Dissolve and remove the metal foil in the portions that are not present to obtain the desired pattern.
  • a method called an additive method is to form a circuit pattern by electroless plating only on a wiring portion.
  • a method of producing a circuit pattern by an additive method using a photoreaction see Japanese Patent Application Laid-Open Nos. 10-209586, e-SS ?, 48-20065, 48-24250, and 48-24250. 48-24255 and others.
  • Japanese Patent Application Laid-Open No. 10-209586 discloses a method in which a desired pattern area is selectively irradiated with light in the presence of oxygen on a polyorganosilane film, a pattern having an SiO bond in the light irradiated area is formed, and then the SiO bond is formed.
  • the organopolysilane film After dissolving the pattern portion using a solvent that dissolves only the pattern portion having, and leaving only the unirradiated portion of the organopolysilane film on the substrate, the organopolysilane film is irradiated with light in the presence of oxygen. Then, an SiO bond is formed on the surface of the organopolysilane film, and a silver salt is catalytically reduced on the SiO bond to form a silver conductive layer.
  • JP-A-46-827 discloses that the reduction of palladium chloride by photo-oxidation of a reducing metal salt causes the deposition of palladium only in a portion not irradiated with light.
  • JP-A-48-24250 perform electroless plating using a free metal formed by photoreduction of a metal salt as a nucleus.
  • Japanese Patent Application Laid-Open No. 58-222592 discloses a method of attaching a catalyst particle only to a pattern portion and then performing electroless plating.
  • these are not reproducible circuit patterns and There are various drawbacks, such as abnormal deposition in the conductive circuit part, and there are many drawbacks in the printed circuit board manufacturing method, and there is much room for improvement.
  • problems such as low density of the plating, extremely large variation of the plating, and formation of an alloy instead of a pure metal.
  • increasing the amount of noble metal salt raises the cost of the catalyst, lowers the adhesion to the substrate, lowers the strength, and may cause problems such as the occurrence of mid-damage.
  • the conductive wiring pattern can also be formed by printing a paste obtained by kneading a noble metal and a resin binder curable by light, heat or electron beam on the substrate by screen printing or the like, and curing the resin binder. It can be formed.
  • the particles must be highly viscous in order to keep the particles in suspension, and must have a suitable pseudoplastic fluidity and thixotropic fluidity to be screen-printable.
  • mixing the organic and inorganic salt components of the ink requires physical milling and mixing with a roll mill or the like.
  • the particle size of the noble metal milled by such a method is 0.5 to 4 m.
  • the composition thus formed is formed into a thin film, film, or plate, and a mask pattern is adhered to the composition, and by irradiating ultraviolet light or visible light, the oxidizing properties of the light-irradiated portion are lost and the pyrrole is polymerized. It is something that does not. However, this method has the problem that it cannot be used as a metal electron circuit because of its low conductivity.
  • Japanese Patent Application Laid-Open No. H11-243273 discloses a method of providing a metal pattern that can be used as a conductive line by depositing a metal colloid having a protective sheath as a precursor on a substrate as a thin film and then irradiating the surface with spatially selective light irradiation.
  • the present invention provides a method for forming a metal wiring, which comprises decomposing or destroying the outer skin to form a metal thin film, and then removing a metal colloid in an unexposed portion.
  • the tetraalkylammonium salt / ethylene oxide which is the outer skin of the metal, must be destroyed with a laser or the like, and the metals must be fused together.
  • An object of the present invention is to use a metal colloid solution composition having extremely excellent dispersion stability and a micro-discharge technique, thereby eliminating the need for complicated steps such as coating and stripping with a resist, and making it possible to produce a semiconductor or nonconductive substrate with a very low level.
  • An object of the present invention is to provide a method for easily forming a fine conductor or semiconductor wiring pattern with high dimensional accuracy.
  • the present invention relates to a compound represented by the general formula: X-HLS-HBS-Y, X-HBP-Y or X-HLP-Y, wherein HLS is a hydrophilic segment, HBS is a hydrophobic segment, HBP is a hydrophobic segment, HLP Represents a hydrophilic segment, and X and Y represent hydrogen, an alkyl group, a phenyl group, a mercapto group, a silanol group, a metal alkoxy, an alkoxy group, a sulfide group, an acetyl group, an acetal group, an aldehyde group, and a thioaldehyde, respectively.
  • the particle size of the colloidal particles such as metal or metal oxide in the metal colloid solution composition of the present invention has a diameter of l to 1000 nm, preferably l to 500 nm, and more preferably 1 to LOOnm.
  • the method for preparing the metal colloid particles is not particularly limited, and a general chemical method or physical method can be used.
  • Chemical method can prepare fine particles with uniform particle size and form fine wiring Suitable for preparing precursors for The chemical method is to aggregate or crystallize metal atoms after reduction of metal ions.
  • Methods for preparing metal colloid particles by a chemical method include a dry-reduction method in which reduction is performed in a vacuum or gas, and a wet-reduction method in which reduction is performed in a solvent.
  • the wet method is generally preferred because the equipment is simple and the operation is easy.
  • a metal salt can be reduced to obtain a metal having a zero atomic value.
  • Colloids prepared by the wet-reduction method are particularly preferred, as they have a smaller particle size and have a narrower particle size distribution than other methods.
  • a polymer protecting agent may be added after reducing the ions, or the polymer protecting agent may be dissolved in a solvent in advance and coexisted with the polymer protecting agent. May be used to reduce the ions. In the latter case, during the process in which the ions are reduced to metal atoms, the hydrophobic portion of the polymer chain is physically adsorbed or chemisorbed to the particle surface as a train by hydrophobic interaction on the metal atom surface. Due to the steric repulsion of the polymer protecting agent adsorbed on the metal atom, excessive aggregation of the colloid is suppressed, and the solvent-philic portion of the polymer protecting agent spreads and disperses in the solvent.
  • the solvent used in the reduction method is not particularly limited as long as it can dissolve the metal salt in water, alcohol, ether, ester, chlorinated hydrocarbon, amine or the like, or a mixed solvent thereof.
  • water, methanol, ethanol, Lower aliphatic alcohols having mild reducing properties such as 2-propanol are preferably used.
  • water, methanol, and ethanol are preferable, and water, a mixture of water and methanol, or a mixture of water and ethanol are more preferable.
  • a method of preparing a colloid using such a reduction method there is disclosed a method of preparing a colloid using silver, gold, and copper salts and using polybierpipididone or polyvinyl alcohol as a polymer protecting agent ( Journal of Applied Polymer Science 44 p.1003 1992, Chemical Society Japan 59 p.367 1986, Journal Colloid and Interface Science 156 p.240 1993).
  • the metal all metals can be used in principle, but a transition metal is preferable, and a transition metal of Group 8 to 11 of the periodic table is more preferable. preferable.
  • Most preferred are iron, cobalt, nickel, copper, ruthenium, rhodium, iridium, palladium, gold, platinum and silver. Also, rhenium can be preferably used.
  • the type of the metal salt of the colloid compound and the acid of the metal in the present invention are not particularly limited, but they must have high solubility in a solvent, and include halides, nitrates, acetates, acetic anhydrides, sulfates, and the like. Acetate and the like. Of these, nitrates and hydrochlorides are particularly preferably used.
  • Suitable metal salts include, for example, chloroplatinic acid, chloroauric acid, silver nitrate, rhodium chloride, palladium chloride, rubidium chloride, copper chloride, iron chloride, anhydrous palladium acetate, copper sulfate and the like.
  • metal colloids of alloys using a mixture of two or more metal salts.
  • a method for preparing copper / platinum and copper / palladium pimetallic metal colloids is disclosed (JOURNAL OF MACROMOLECULAR SCIENCE CHEMISTRY A p. 1225-1238 1990, CHEMISTY LETTERS p. 1611-1614 1993).
  • Examples of metals capable of forming the core-shell structure include CdSe / ZnS, Au / Pt, Pt / Pd, and Cu / Pd (Chemical Review 87, p.877 1987, Journal of American Chemical Society 112. 1327 1990).
  • the reduction operation of metal salts includes chemical methods, photochemical methods, thermal decomposition methods, electrochemical methods, and ultrasonic methods.
  • the chemical method is carried out by contacting with an appropriate reducing agent.
  • the reducing agent and the metal are mixed in almost stoichiometric amounts.
  • the reducing agent may be an inorganic reducing agent or an organic reducing agent.
  • Examples of the reducing agent include formamide, hydrogen, alcohol, formaldehyde, sodium citrate, hydrazine, alkylborane, boron compounds and urea.
  • alcohols have high solubility of the above salts and can be used as a solvent. It is preferable because it functions.
  • boron compounds include sodium borohydride and lithium borohydride, with sodium borohydride being highly preferred. Reduction is usually performed in the presence of a polymer without the addition of an acid or base.
  • the proportion of total solids in the reducing solution is generally 10-40% by weight, preferably 15-30% by weight, most preferably 15-25% by weight.
  • the colloid solution composition of the present invention contains 0.5 to 50% by weight of metal particles in the solid content. Preferably. More preferably 1 one 30% by weight, particularly preferably 5- 20 by weight 0 /. Metal particles.
  • the proportion of the polymer in the solid content of the composition is generally 50 to 99.5% by weight, preferably 70 to 99% by weight. /. , Most preferably 80-95 weight 0 /. It is.
  • the photochemical reduction method is performed by irradiating the metal salt solution with high-energy radiation, visible light, ⁇ -rays, particularly ultraviolet rays.
  • the preparation of colloids by a physical method is a method in which metal nanoparticles are prepared by, for example, vacuum evaporation, trapped at a low temperature, and then stabilized with a polymer protective agent.
  • metal nanoparticles are prepared by, for example, vacuum evaporation, trapped at a low temperature, and then stabilized with a polymer protective agent.
  • particle size reduction There is a limit to particle size reduction, and the particle size distribution is often wide.
  • gold and platinum which have high malleability and / or ductility and are not easily formed into fine particles by physical pulverization, are preferably prepared by the former chemical method.
  • the above-mentioned polymer protective agent may be added after the metal is finely pulverized, or the polymer protective agent may be dissolved in a solvent in advance and then pulverized.
  • the colloid preparation method includes the above-mentioned chemical method and physical method.
  • the polymer protectant absorbs the hydrophobic part of the polymer chain as a train on the particle surface by hydrophobic interaction, and the solvent-philic part in the polymer chain forms a loop or tail. It spreads in the solvent and can be stably dispersed.
  • the method of preparing a colloidal particle by a chemical method such as a reduction method in the presence of a polymer protecting agent has a small number average particle diameter, a narrow particle size distribution, and It is suitable because of its high dispersion stability.
  • the polymer protecting agent may be added after the ion reducing operation.
  • metal oxide in the metal oxide colloid arsenic one ⁇ 1 2 0 3, ⁇ ⁇ a -A1 2 0 3, - AIOOH, r - AIOOH, - ⁇ 1 ( ⁇ ) 3, ⁇ _ Al (OH) 3 , BeO, CdO, Cd (OH ) 2, Co (OH) 2, Cu (OH) 2, CuO, Cr 2 0 3, Fe (OH) 2, Fe 3 O 4, - Fe 2 0 3, r - Fe 2 0 3, - FeOOH, r - FeOOH, Pb (OH) 2, MgO, Mg (OH) 2, Mn (OH) 2, HgO, NiO, Ni (OH) 2, Pu0 2, SiO, Th0 2, Sn0 2, Ti0 2, W0 3, V 3 0 8, Y 2 0 3, ZnO, Zr0 2, La 2 O 3, Ca ⁇ La ⁇ TaO ⁇ N , and the like.
  • X-HLS-HBS-Y, X-HBP-Y or X-HLP-Y of the present invention is a metal, a composite metal oxide, a solid solution comprising at least two kinds of metals, or a core-shell as a polymer protective agent.
  • the colloid of dispersion-stabilized fine particles adsorbed on the surface of a metal class having a structure can be prepared by the method described above.
  • the hydrophilic segment HLS and the hydrophilic segment HLP in the polymer protective agent are preferably polyethylene glycol, polypropylene glycol, polyvinyl alcohol, poly (meth) acrylic acid, polyvinyl pyridine, polyvinyl pyrrolidone, polyacrylamide, polydimethylacrylamide, poly Methyl vinyl ether, a copolymer thereof or a derivative thereof, and the hydrophobic segment HBS and the hydrophobic segment HBP are preferably polylactide, polyglycolide, poly (butyrolactone), poly (valerolactone), polypropylene glycol, polyglycol.
  • the polymer protecting agent is obtained by bonding an amino group, a mercapto group, a silanol group, an acetyl group, an acetal group or a derivative thereof to one end or both ends of polyethylene dalicol.
  • the polymer protective agent is limited to either hydrophilic or water-phobic, and the solvent for redispersing the prepared metal colloid fine particles during preparation or when preparing the same colloid is used. It is limited to either hydrophilic solvents or hydrophobic solvents.
  • the present invention has devised a method of forming fine wiring having high dimensional accuracy on substrates of various materials using the above-mentioned dispersion-stable colloid composition. That is, according to the present invention, the contained metal, metal oxide, conductive polymer or conductive colloid can be approached or contacted at a distance of several rnn, and non-quantum or quantum electrons can be brought into contact. Conduction due to movement can occur.
  • the size of the colloidal particles prepared by the above method is less than 50 nm or less than 100 nm, and quantum conduction occurs.
  • the conductivity can be optimized by changing the compounding ratio of each compound.
  • the dopant can be added to the solution in advance.
  • a dispersion-stabilized metal colloid solution obtained by bonding the polymer protective agent of the present invention to a metal having zero oxidation number is applied to the substrate by means of an inkjet or other device capable of finely controlling the discharge amount. By coating and depositing on the substrate and curing it together with the precursor of the conductive polymer contained in the colloid solution, it is possible to obtain a wiring having high conductivity and high mechanical strength.
  • metal all metals can be used in principle, but a transition metal is preferable, and a transition metal of Groups 8 to 11 of the periodic table is more preferable. Most preferred are iron, cobalt, nickel, copper, ruthenium, orifice, rhenium, iridium, palladium, gold, platinum and silver.
  • the colloid used for forming the conductor or semiconductor pattern is iron, manganese, chromium, cobalt, nickel, copper, zinc, palladium, molybdenum, tungsten, ruthenium, osmium, iridium, platinum, silver prepared by the method described above.
  • Gold, germanium, tin, gallium, indium, and the like preferably a colloid comprising palladium, gold, silver, nickel or copper.
  • a metal oxide colloid having an oxidation number other than zero as described above may be used. It is well known that even oxides can be reduced by a reducing agent or electrical reduction to reduce the oxidation number to zero.
  • the metal oxide is an oxide of the metal.
  • cadmium sulfide, titanium oxide, and silicon oxide, which are semiconductors, may be used as the metal or metal oxide.
  • Silver is generally known to cause a change in electrical properties due to migration, and thus silver may be used in a mixture with other metals or metal oxides.
  • a colloid composed of an alloy by mixing a plurality of metal colloids or metal oxide colloids, or a colloid composed of a solid solution thereof may be used.
  • the mixture may be sintered to form an alloy or a solid solution.
  • silver Z palladium, silver / platinum, platinum Z gold / silver may be used for the purpose of chemical stability.
  • a single copper microparticle colloid easily reacts with oxygen and is unstable, but becomes stable when alloyed with a noble metal such as palladium.
  • the molecular weight of the polymer protective agent in the colloid solution composition of the present invention can be 100 or more, preferably 100 to: 100,000, more preferably about 200 to 20,000.
  • the colloid solution composition and the conductor or semiconductor pattern forming ink of the present invention contain at least alcohol, surfactant, preservative and chelating agent.
  • One type can be included. Specifically, diethylene glycol, triethylene glycol, tetraethylene glycol, dipropylene glycol, propylene glycol, polyethylene glycol, polypropylene glycol, ethylene glycol, propylene glycol, trimethylene glycol, butylene glycol, 1 , 2,6-hexanetriol, hexylene glycol, glycerin, ethylene glycol monomethyl (or ethyl) ether, diethylene glycol monomethyl (or ethyl) ether, triethylene glycol monomethyl (or ethyl) ether, Triethylene glycol dimethyl (or ethyl) ether, tetraethylene glycol dimethyl (or ethyl) ether, etc., 0.1 to 45% by weight of alcohol, preferably Ku may be added 1 to 40% by weight.
  • the solvent of the colloid solution composition of the present invention and the conductor or ink for forming a semiconductor pattern is not particularly limited, and the dispersion of colloid such as water, alcohol, ether, ester, chlorinated hydrocarbon, amine and the like and a mixed solvent thereof is used.
  • a high-performance solvent can be suitably used.
  • the colloid solution composition and the conductor or semiconductor pattern forming ink of the present invention contain a curable compound or a thermoplastic resin which can be cured by irradiating light, heat or electron beam energy to cause a polymerization reaction.
  • a curable compound or a thermoplastic resin which can be cured by irradiating light, heat or electron beam energy to cause a polymerization reaction.
  • a compound that can be cured by irradiation with light, heat or electron beam energy is coated on a semiconductor or non-conductive substrate and then cured by irradiation with light, heat or electron beam energy, and the curable compound is cured. After curing, it becomes a conductive polymer.
  • the colloid solution composition and the conductor or the ink for forming a semiconductor pattern contain a polymerization accelerator of a precursor of a dopant or a polymer cured product for improving the electron conductivity of the conductive polymer. You can also.
  • the colloid solution composition and the conductor or semiconductor pattern forming ink of the present invention can also contain a conductive colloid and a conductive polymer soluble in a solvent.
  • the conductive polymer having solubility in the solvent is an external dopant type. However, it may be a self-punting type. Specifically, the following equation
  • Poly (naphtho [2,3-c] pyrrole-1,3-diyl-2-yl- (sodium 2'-ethanesulfonate)) and the like can be used.
  • the terminal X and Y of the polymer of the polymer protecting agent in the colloid solution composition of the present invention are hydrogen, alkyl group, phenyl group, mercapto group, silanol group, metal alkoxy, alkoxy group, sulfide group, acetyl, Group, acetal group, aldehyde group, thioaldehyde group, oxo group, thioxo group, hydroperoxy group, amino group, imino group, hydrazino group, carpoxy group, thiocarpoxy group, dithiocarpoxy group, sulfo group, sulfino group, sulfeno group Oxypropyl, haloformyl, .99amoyl, hydrazinocarbonyl, amidino, cyano, nitrite, isocyano, cyanate, isocyanato, thiocyanato, isothiocyanato, methyacryloy
  • the metal or metal oxide can be adsorbed by the mercapto group.
  • the metal or metal oxide can be adsorbed by the silanol group, and is preferably palladium, cadmium sulfide, titanium oxide, or calcium oxide. Is prime.
  • the colloid solution is coated by spin coating, dipping, casting, vacuum deposition, Langmuir-Blodgett, or other method. By forming a thin film, a thin film having a function as a photocatalyst can be formed.
  • the physical shape need not be a thin film but may be a linear shape.
  • An ink jet printer that can control a very fine ejection of several pi (picoliter) can be used for forming the fine wire. Further, it is possible to use a discharge device such as that used in a capillary electrophoresis analyzer.
  • a discharge device such as that used in a capillary electrophoresis analyzer.
  • metal particles In order to obtain high conductivity, it is necessary for metal particles to be close to each other, more preferably in contact. To this end, it is desirable to reduce or eliminate the amount of organic compounds that cause a decrease in conductivity with respect to metals. However, if the amount of the organic compound relative to the metal or metal oxide is too small, sufficient mechanical strength cannot be obtained, and the adhesion to the substrate also decreases.
  • the amount ⁇ of the conductive substance relative to the organic compound is greater than the critical volume fraction £ e in the theory of percolation, that is, ⁇
  • the weight of the metal or metal oxide relative to the organic compound remaining after evaporation of the solvent is from 10% to 100% by weight, preferably 40 ° /. ⁇ : 100%.
  • the concentration of the metal or metal oxide fine particles may be at least the critical micelle concentration, and is at least 5%, preferably at least 20%, most preferably at least 50% by weight relative to the solvent.
  • the number of conductive paths can be increased by decomposing or removing some or all of the remaining organic compounds by light, heat or chemical treatment.
  • the percentage by weight is less than 90%, preferably less than 80% and more preferably less than 30%.
  • organic compounds can be reduced or removed by a method such as heating. Heating in an oxygen-free state can prevent the metal from becoming an oxide. The heating is at 200 ° C, preferably 500 ° C, more preferably about 800 ° C or more.
  • the colloid solution composition and the conductor or semiconductor pattern forming ink of the present invention can contain a curable compound or a thermoplastic resin which can be cured by irradiating light, heat or electron beam energy to cause a polymerization reaction.
  • a curable compound an ultraviolet curable resin, a thermosetting resin, an electron beam curable resin, or the like can be used.
  • UV-curable resins include photopolymerizable prepolymers, photopolymerizable monomers, photoinitiators, and sensitizers.
  • the photopolymerizable prepolymer polyester acrylate, polyurethane acrylate, polyester urethane acrylate, epoxy acrylate, polyol acrylate and the like can be used.
  • Photopolymerizable monomers include 2-ethylhexyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, acrylic acid, isobutyl acrylate, tributyl acrylate, lauryl tridecyl acrylate , Stearyl acrylate, tetrahydrofurfuryl acrylate, cyclohexyl acrylate, benzyl acrylate, 2-hydroxy-3-phenyloxypropyl acrylate, 2-hydroxyethyl acrylate , 2-hydroxypropyl acrylate, 2-methoxyethyl acrylate, phenoxyshetyl acrylate, ethoxydiethylene glycol acrylate, monofunctional acrylate such as methoxydipropylene glycol acrylate, 1,3-butanediol Luziacrylate, Neo Pentyl diol diacrylate, 1,4-butane diol diacrylate, 1,6-hexan
  • photoinitiators examples include acetophenone, benzophenone, Michler's ketone, benzyl, benzoin, benzoin isobutyl ether, benzyl methyl ketal, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-dimethyl-1-phenylpropane-1- On, 1- (4-isopropylphenyl) -2-hydroxy-2-methylpropan-1-one, azobisisobutyl nitrile, benzoyl peroxide, di-tert-butyl peroxide can be used. .
  • sensitizers include benzoin isopropyl ether, n-butylamine, di-n-butylamine, triethylamine, isoamyl P-dimethylaminobenzoate, and ethylaminoethyl methyl acrylate.
  • electron beam-curable resins include polyvinylidene fluoride, terminal bier esters, unsaturated polyester ZN oxohydrocarbon-substituted acrylamide, halogen-containing olefin-type unsaturated polyester, alkyd resin, modified polyester and blend, unsaturated polyester, acrylic Epoxy soybean oil ammine, Epoxyester ester saturated alkyd, Chlorinated paraffin and acrylate, Z acrylate oil, Epoxy, Polyol rubbamate Unsaturated monomer, Polyester type oligo (meth) acrylate, Linear copolymer of glycidol, Aromatic polysulfone , Diacrylates and unsaturated olefins.
  • the electron beam crosslinking resin examples include polyglycidyl methacrylate (PGMA), polyglycidyl methacrylate methacrylate, maleic acid adduct of polyglycidyl methacrylate, chloromethylated polystyrene, polydiaryl orthophthalate, epoxidized polybutadiene, Polyethyl acrylate- ⁇ -chloro acrylonitrile, polystyrenetetrathiofulvalene, polymethylmeth And acrylate acrylates.
  • PGMA polyglycidyl methacrylate
  • maleic acid adduct of polyglycidyl methacrylate chloromethylated polystyrene
  • polydiaryl orthophthalate epoxidized polybutadiene
  • Polyethyl acrylate- ⁇ -chloro acrylonitrile Polystyrenetetrathiofulvalene
  • polymethylmeth And acrylate acrylates examples include polyglycid
  • thermosetting resin epoxy, phenol, polyimide, and urea compounds
  • an appropriate resin may be selected according to the required characteristics such as adhesion to the substrate.
  • thermoplastic resin a general acrylic compound or polyester compound can be used.
  • Figure 1 is a chart showing the results of proton NMR measurement of the polymeric protective agent.
  • Figure 2 is a graph of the UV absorption spectrum of the metal colloid in a THF solution.
  • Figure 3 is a graph of the UV absorption spectrum of the metal colloid after three centrifugation operations.
  • Fig. 4 is a chart showing the measurement results of the zeta potential of the PEG silver fine particles.
  • the polymer (5) shown in the following reaction formula was obtained by reacting with potassium O-ethyl dithiocarbonate at room temperature for 3 hours. Thereafter, a polymer having a mercapto group at the terminal (6) shown in the following reaction formula was obtained by the same reaction with propylamine in THF.
  • This colloidal solution composition was coated on a substrate with a doctor blade and dried and cured in the same manner.
  • the heterobifunctional PEG (1) shown in the following reaction formula is anion-polymerized. Synthesized. Furthermore, the polymer (2) shown in the following reaction formula was obtained by reacting with O-ethyl potassium dithiocarbonate in THF at room temperature for 3 hours. After that, the reaction with propylamine in THF also yielded a heterobifunctional PEG (3) having a mercapto group at the end, as shown in the following reaction formula.
  • FIG. 1 shows the proton NMR measurement results of the polymers (1) to (3) shown in the above reaction formula obtained by the above method.
  • silver nitrate synthesized by the above method 10 g
  • l.Og of sodium borohydride was added to this to prepare a yellow-brown colloidal solution.
  • Excessive Acetal-PEG-SH was removed by centrifugation (gravitational acceleration: 42.000 x 9.8 m / sec 2 , 30 minutes). The solution remaining after centrifugation was dropped onto 3 mL of THF and stirred. The absorption spectra of these samples were taken and their characteristics were analyzed. The results are shown in Fig. 2.
  • the UV-vis spectrum of the silver particles re-dispersed in a THF solution after centrifugation, and the UV spectrum of unmodified silver particles (b) are as follows: It was confirmed that a large absorption peak at a wavelength of 500 nm or more based on the aggregation of particles was exhibited. Acetal-PEG-OH (c) did not have a large peak at a wavelength of 500 nm or more like the UV spectrum of unmodified silver particles, but the overall peak shifted to higher wavelengths and the particle dispersion was somewhat higher. It was confirmed that it had become unstable.
  • the part containing the film was dried with far-infrared rays and cooled to room temperature, and then irradiated with ultraviolet light for 10 minutes using a metal halide lamp MO3-L21 (Lamp output: 80 WZcm 2 ) manufactured by Kyushu Co., Ltd., and photopolymerized to form a conductor wiring pattern. did. The volume resistance value of this conductor wiring pattern was measured.
  • the colloidal solution composition was coated on a substrate with a doctor blade and dried and cured in the same manner.
  • the solution was discharged onto a substrate with a phosphor mixer MJ8000C, and the substrate was covered with a thin cast film composed of the above solution. Next, the part including the cast film on this substrate was dried with far infrared rays to form a conductor wiring pattern. The volume resistance value of this conductor wiring pattern was measured.
  • This colloid solution composition was coated on a substrate with a doctor blade, and dried and cured in the same manner.
  • a wiring pattern was printed on a substrate using a stainless steel 400-mesh screen printing plate made of Nippon Acheson conductive silver paste ink ED975SS, and cured at 135 ° C for 60 minutes.
  • the volume resistance value of the prepared silver paste conductor was measured.
  • the line widths of the wiring patterns of Examples 1 to 4 and Comparative Example 1 were measured with a Keyence Corp. laser-focus displacement meter LT8020.
  • the volume resistance was measured with a digital multimeter tester manufactured by Mitsubishi Chemical Corporation and calculated by converting the film thickness. Table 1 shows the results of these measurements.
  • the metal colloid solution composition of the present invention has extremely excellent dispersibility, particularly when a noble metal is used, has a very small particle size.
  • the conductor or semiconductor pattern forming ink of the present invention comprising this colloid solution composition is: An electronic substrate can be manufactured by easily forming a fine wiring pattern that can be a conductor in which metals come close to or in contact with each other on a semiconductor or nonconductor substrate.

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  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
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  • Manufacturing Of Printed Wiring (AREA)

Abstract

L'invention concerne un motif conducteur ou semi-conducteur formé sur un substrat semi-conducteur ou non conducteur par éjection d'une solution sur une surface du substrat, la solution servant de précurseur d'un conducteur ou d'un semi-conducteur, et comprenant un métal ou un colloïde d'oxyde métallique composite produit par liaison d'un composé polymère doté d'un groupe fonctionnel présentant une forte adsorption physique ou chimique à un métal ou un oxyde métallique, servant d'agent de protection, à une terminaison ou aux terminaisons d'un copolymère bloc renfermant un bloc hydrophile et un bloc hydrophobe, un composé qui peut sécher lors d'une irradiation par énergie lumineuse, thermique ou d'un faisceau d'électrons, et un solvant. L'éjection de la solution s'effectue selon un motif souhaité au moyen d'un éjecteur qui peut commander délicatement le jet d'une imprimante à jet d'encre. Une partie du substrat revêtu de la solution est ensuite irradiée par une énergie lumineuse, thermique ou d'un faisceau d'électrons, ce qui durcit ladite partie.
PCT/JP2001/006655 2000-08-03 2001-08-02 Composition de solution colloidale metallique et conducteur ou encre destine a la formation d'un motif semi-conducteur la renfermant, et procede de formation d'un motif conducteur ou semi-conducteur Ceased WO2002018080A1 (fr)

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JP2005097345A (ja) * 2003-09-22 2005-04-14 Konica Minolta Medical & Graphic Inc インクジェットインクおよびこれを用い作製した非接触通信機能を有するｉｃ基体
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JP2005229109A (ja) * 2004-02-10 2005-08-25 E I Du Pont De Nemours & Co インクジェット印刷可能な厚膜インク組成物および方法
WO2005080032A1 (fr) * 2004-02-20 2005-09-01 Kazunori Kataoka Procédé de fabrication de colloïde de fer, et micelle polymère porteuse de colloïde de fer
WO2005108507A1 (fr) * 2004-05-07 2005-11-17 Canon Kabushiki Kaisha Composition, procede de formation d’image employant la composition, et procédé d'élaboration de motif électroconducteur
JP2006009120A (ja) * 2004-06-29 2006-01-12 Asahi Kasei Corp 金属微粒子分散体
JP2006183092A (ja) * 2004-12-27 2006-07-13 Sumitomo Electric Ind Ltd 合金微粒子の製造方法とそれによって製造される合金微粒子および金属コロイド溶液
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