Method for forming fine copper particle sintered product type of electric conductor having fine shape, and process for forming copper fine wiring and thin copper film by applying said method
First Claim
1. A process for forming a copper-based fine pattern consisting of a sintered product layer made of copper nano-particles sintered with each other, which process comprises the steps of:
- drawing a layer coated on a substrate, which layer has a fine pattern, by using a dispersion containing copper oxide nano-particles or copper nano-particles provided with a surface oxide film layer, which particles have an average particle diameter of 1 to 100 nm, together with a dispersion medium thereof andsubjecting the copper oxide nano-particles or the copper nano-particles provided with the surface oxide film layer contained in the coated layer drawn by using the dispersion to a reducing treatment, wherein the copper oxides or surface oxide film layer are reduced at a heating temperature selected form the range of 180°
C. to 300°
C. by using an organic compound having reducing activity, and further a baking treatment wherein the copper nano-particles resulting from the reducing treatment are baked at the heating temperature selected from the range of 180°
C. to 300°
C. to form a sintered product layer made of the copper nano-particles in the fine pattern,wherein the sintered product layer made of copper nano-particles that is formed by the process consists of the copper nano-particles sintered with each other, the coated layer drawn by using the dispersion contains the dispersion medium, the dispersion medium is an organic solvent, and said reducing treatment and the baking treatment that is carried out by heating at a heating temperature selected from the range of 180°
C. to 300°
C. in single stage which is conducted by heating the copper oxide nano-particles or the copper nano-particles with the surface oxide film layer contained in the coated layer in the presence of the organic compound having reducing activity at the heating temperature selected from the range of 180°
C. to 300°
C., thereby giving rise to the action of said organic compound having reducing activity on the copper oxide nano-particles or the surface oxide film layer.
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Accused Products
Abstract
The present invention provides a process for forming a copper fine particle sintered product type of a fine-shaped electric conductor showing superior electroconductivity, which comprises steps of drawing a fine pattern with the use of a dispersion containing the copper fine particles having a surface oxide film layer, conducting a treatment for reducing the copper fine particles with the surface oxide film layer or copper oxide fine particles included in the pattern at a comparatively low temperature, and baking the resultant copper fine particles. Specifically, the process carries out the processes of; applying a dispersion containing the copper fine particles having the surface oxide film layer thereon or the copper oxide fine particles with an average particle diameter of 10 μm or smaller onto a substrate; and then performing a series of the heat treatment steps of heating the particles in the coated layer at temperature of 350° C. or lower under an atmosphere containing a vapor and a gas of a compound having reducibility to reduce the oxide film by a reduction reaction which used the compound having reducibility as a reducing agent, subsequently repeating a heat treatment combining an oxidizing treatment of a short time with a re-reducing treatment, and sintering the resultant copper fine particles with each other to form a layer of the sintered product.
3 Citations
30 Claims
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1. A process for forming a copper-based fine pattern consisting of a sintered product layer made of copper nano-particles sintered with each other, which process comprises the steps of:
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drawing a layer coated on a substrate, which layer has a fine pattern, by using a dispersion containing copper oxide nano-particles or copper nano-particles provided with a surface oxide film layer, which particles have an average particle diameter of 1 to 100 nm, together with a dispersion medium thereof and subjecting the copper oxide nano-particles or the copper nano-particles provided with the surface oxide film layer contained in the coated layer drawn by using the dispersion to a reducing treatment, wherein the copper oxides or surface oxide film layer are reduced at a heating temperature selected form the range of 180°
C. to 300°
C. by using an organic compound having reducing activity, and further a baking treatment wherein the copper nano-particles resulting from the reducing treatment are baked at the heating temperature selected from the range of 180°
C. to 300°
C. to form a sintered product layer made of the copper nano-particles in the fine pattern,wherein the sintered product layer made of copper nano-particles that is formed by the process consists of the copper nano-particles sintered with each other, the coated layer drawn by using the dispersion contains the dispersion medium, the dispersion medium is an organic solvent, and said reducing treatment and the baking treatment that is carried out by heating at a heating temperature selected from the range of 180°
C. to 300°
C. in single stage which is conducted by heating the copper oxide nano-particles or the copper nano-particles with the surface oxide film layer contained in the coated layer in the presence of the organic compound having reducing activity at the heating temperature selected from the range of 180°
C. to 300°
C., thereby giving rise to the action of said organic compound having reducing activity on the copper oxide nano-particles or the surface oxide film layer. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 18, 26, 27, 28)
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12. A process for forming a copper thin-film layer consisting of a sintered product layer made of copper fine particles sintered with each other, wherein the process comprises the steps of:
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drawing a layer coated on a substrate by using a dispersion containing copper oxide fine particles or copper fine particles provided with a surface oxide film layer, which particles have an average particle diameter of 10 μ
m or less, together with a dispersion medium thereof andsubjecting the copper oxide fine particles or the copper fine particles with the surface oxide film layer contained in the coated layer drawn by using the dispersion to a reducing treatment wherein the copper oxides or the surface oxide film layer are reduced at a heating temperature selected form the range of 250°
C. to 350°
C. by using an organic compound having reducing activity, and further to a baking treatment wherein the copper fine particles resulting from the reducing treatment are baked at the heating temperature selected form the range of 250°
C. to 350°
C. to form a sintered product layer made of the copper fine particles,wherein the sintered product layer made of copper fine particles sintered with each other consists of the copper fine particles sintered with each other, the coated layer drawn by using the dispersion contains the dispersion medium, the dispersion medium is an organic solvent, said reducing treatment and the baking treatment comprise the following two steps that are executed sequentially in a single process at the heating temperature selected from the range of 250°
C. to 350°
C.;a first treatment step of heating the copper oxide fine particles or the copper fine particles provided with the surface oxide film layer contained in the coated layer for duration of 1 min. to 15 min. at the heating temperature selected from the range of 250°
C. to 350°
C. in the presence of an organic compound having reducing activity to give rise to the action of said organic compound having reducing activity thereon, and thereby reducing the copper oxides composing the copper oxide fine particles or the copper fine particles provided with the surface oxide film layer to provide copper fine particles; anda second treatment step of subjecting said copper fine particles obtained in the first treatment step to a combined treatment of oxidation/re-reduction at least one time, which includes a stage of subjecting the copper fine particles to a surface oxidization treatment by heating for 30 seconds or shorter at the heating temperature selected from the range of 250°
C. to 350°
C. under an atmosphere containing oxygen to give rise to the action of oxygen thereon, and then a stage of subjecting the copper fine particles, which have undergone the surface oxidization treatment, to a re-reduction treatment by heating the particles for 30 seconds or longer but 300 seconds or shorter at the heating temperature selected from the range of 250°
C. to 350°
C. under an atmosphere containing gas or vapor of said organic compound having reducing activity to give rise to the action of said organic compound having reducing activity thereon. - View Dependent Claims (13, 14, 15, 16, 17, 19, 20, 21, 29)
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22. A process for forming a copper thin-film layer consisting of a product layer made of copper fine particles sintered with each other, wherein the process comprises the steps of:
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drawing a layer coated on a substrate by using a dispersion containing copper oxide fine particles or copper fine particles provided with a surface oxide film layer, which particles have an average particle diameter of 10 μ
m or less, together with a dispersion medium thereof and subjecting the copper oxide fine particles or the copper fine particles with the surface oxide film layer contained in the coated layer drawn by using the dispersion to a reducing treatment wherein the copper oxides or the surface oxide film layer are reduced by using a hydrogen molecule at a heating temperature selected from the range of 250°
C. to 350°
C., and further to a baking treatment wherein the copper fine particles resulting from the reducing treatment are baked at the heating temperature selected from the range of 250°
C. to 350°
C. to form a sintered product layer of the copper fine particles,wherein the sintered product layer made of copper fine particles sintered with each other consists of the copper fine particles sintered with each other, the coated layer drawn by using the dispersion contains the dispersion medium, the dispersion medium is an organic solvent, said reducing treatment and the baking treatment comprise the following two steps that are executed sequentially in a single process at the heating temperature selected from the range of 250°
C. to 350°
C.;a first treatment step of heating the copper oxide fine particles or the copper fine particles provided with the surface oxide film layer contained in the coated layer for duration of 1 min. to 15 min. at the heating temperature selected form the range of 250°
C. to 350°
C. in the presence of the hydrogen molecule to give rise to the action of said hydrogen molecule thereon, and thereby reducing the copper oxides composing the copper oxide fine particles or the copper fine particles provided with the surface oxide film layer to provide copper fine particles; anda second treatment step of subjecting said copper fine particles obtained in the first treatment step to a combined treatment of oxidation/re-reduction at least one time, which includes a stage of subjecting the copper fine particles to a surface oxidization treatment by heating for 30 seconds or shorter at the heating temperature selected from the range of 250°
C. to 350°
C. under an atmosphere containing oxygen to give rise to the action of oxygen thereon, and then a stage of subjecting the copper fine particles, which have undergone the surface oxidization treatment, to a re-reduction treatment by heating the particles for 30 seconds or longer but 300 seconds or shorter at the heating temperature selected from the range of 250°
C. to 350°
C. under an atmosphere containing said hydrogen molecule to give rise to the action of said hydrogen molecule thereon. - View Dependent Claims (23, 24, 25, 30)
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Specification