Printing composition for obtaining electroconductive coatings based on silver particles dispersed in water, its application for obtaining electroconductive coatings, method of obtaining current-conductive paths and substrate with electroconductive coating

FIELD: chemistry.

SUBSTANCE: invention relates to compositions for obtaining electroconductive coatings on substrates surface. Described is a printing composition for obtaining the electroconductive coatings based on silver particles dispersed in water. The composition contains: a) from 5 to 40 wt.p. of metal silver particles with an effective diameter from 10 to 150 nm, with the silver particles having bimodal distribution of particles by sizes; from 50 to 99.5 wt.p. of water and, if necessary, to 30 wt.p. of a solvent; c) from 0.01 to 15 wt.p. of a dispersing agent; d) from 0 to 5 wt.p of additives; e) from 0 to 5 wt.p. of electroconductive, if necessary, water-soluble, polymers; f) from o.5 to 5 wt.p. of a thickening agent; g) from 30 to 70 wt.p. of silver particles or silver-coated copper particles with an effective diameter from 500 nm to 10 mcm. The composition has a viscosity, at least, 1 Pa·s. Also described is the application of the composition for obtaining the electroconductive coatings, method of obtaining current-conductive paths and a polymer substrate with the electroconductive coating from the claimed composition.

EFFECT: invention provides an effective elctroconductivity of electroconductive structures on thermally stable surfaces with the application of offset printing and screen printing.

15 cl, 2 ex

 

The invention relates to compositions for obtaining structures of electrically conductive structures on surfaces, in particular, to a printing composition to obtain a conductive coating on the basis of the dispersed water particles of silver, its application to obtain a conductive coating, method for producing the conductive tracks and the substrate with a conductive coating.

There is a critical need for electrically conductive structures on the surfaces of objects with poor surface conductivity. In terms of conductivity, for example, applications in the integration of electrical circuits in an electronic component using a printing material held on the surface of the structural lamentablemente, is desirable. This makes it possible to minimize costly problem of the connection elements with separate circuits. In particular, special interest is the printing on the surface of elastic materials with conductive paths.

Freedom of configuration of the entire structural element with a flexible part should no longer be exposed to powerful effect provided by the schema.

In the technique has long been known application of conductive paths made of copper. However, their deposition on the surface is possible only requiring the deposition method and trawl the deposits.

Further development is electrically conductive paste (conductive silver), which can subsequently be applied on the surface and can be used for contact.

Of particular interest is the printing on polymeric materials. In the printing process, in which the surface becomes conductive, the surface of the substrate should not be heated above the softening temperature of the material surface (for example, the glass transition temperature of the polymer surface). In addition, you cannot use any solvent which dissolves or softens the surface.

By known methods, whereby on the surface of low cost and high productivity can be applied patterns are silk-screen printing or offset printing. However, both these methods require other systems used printed materials. So, the specialist is known that the ink or paint that should be used in these printing methods, demands, at least to the viscosity of the printing ink. In order to achieve good printing results, the viscosity should be in the region above 1 PA·S.

In patent applications U.S. US-A-5882722 and US-A-6036889 described conductive compositions containing metal particles, the product of the preceding stage and an organic solvent, which form the electric is provodnye patterns, only when the sintering temperature is from 200°C. These known compositions have a viscosity of about 10 PA·C. Although the data structures and can be used for the described printing methods (screen printing, offset printing), however, due to the required high temperature sintering of their applicability for use on surfaces of polymers is limited.

In the descriptions to the international application WO 2003/038002 and patent applications U.S. US-A-2005/0078158 describes compositions with silver nanoparticles stabilized, among other things, natrocarbonatite-cellulose. Although these publications and describes the need for further processing, for example, heat treatment or treatment with flocculant, however, the temperature of processing, or the conductivity obtained from the composition of the microstructures is described. In addition, does not reveal the exact size distribution used and the obtained nanoparticles, while the domain size is less than 100 nm. The content of silver particles described compositions is not more than 1.2 wt.%. For the intended inkjet method of applying the required viscosity of the ink of the printed composition is about 10 MPa·S. Therefore, the composition is hardly acceptable for screen printing or offset printing.

In the European patent EP 1586604 described silver paste consisting of epoxy resin, flakes and silver nanoparticles sulfur is RA. After printing or coating on the surface of the substrate circuit Board and the subsequent heat treatment this paste forms an electrically conductive film. When the sintering temperature above 200°C is reached the resistance less than 5·105Om/see Such a high sintering temperature severely limits the choice to be printing a polymeric substrate.

In the international application WO 2008/031015 published an aqueous composition containing flakes of silver. When using this composition can be achieved at 120°C conductivity of 0.022 Ohms/square.

The firm HARIMA offers a series of products NP Series Nano-Paste, which is a conductive silver ink on the basis of nanoparticles with low viscosity, HARIMA. However, HARIMA requires a sintering temperature 210-230°C.

There has long been an unresolved problem to obtain a conductive composition that, when used in elementary silver gives you the opportunity to receive electrically conductive patterns on a particularly thermounstable surfaces with offset printing and silk screen printing. Low temperatures in this regard include, for example, a temperature below the glass transition temperature of the polymer surface (PVC ~80°C).

The problem is solved in this invention contains a silver compound, which may be deposited on powernotebooks silk, flexo, gravure or offset printing and can specalise by further heat treatment at a temperature of ≤140°C, if possible, less than 100°C to obtain a conductive structures.

The object of the invention is a printing composition to obtain a conductive coating on the basis of the dispersed water particles of silver, containing at least:

a) from 5 to 40 wt.h. metallic silver particles with an effective diameter of not more than 150 nm, preferably not more than 100 nm, particularly preferably from 20 to 80 nm, most preferably from 40 to 80 nm, specific lateralisation spectroscopy, and the silver particles are, in particular, a bimodal distribution of particle size;

b) from 50 to 99.5 wt.h. water and, if necessary, up to 30 wt.h. solvent;

c) from 0.01 to 15 wt.h., at least one, especially polymeric dispersant;

d) from 0 to 5 wt.h. additives, preferably from 0.5 to 5 wt.h., most preferably from 1 to 4 wt.h. supplements;

e) from 0 to 5 wt.h. conductive, optionally, water-soluble polymer, preferably from 0.5 to 5 wt.h., most preferably from 1 to 4 wt.h. conductive polymer;

moreover, the composition contains additionally

f) from 0.5 to 5 wt.h., preferably from 1 to 4 wt.h. thickener and

g) from 30 to 70 wt.h. metal tactics effective diameter of not more than 10 μm, especially from 500 nm to 10 μm, preferably, silver particles or copper particles coated with silver,

and has a viscosity of at least 1 PA·S.

The sum of the mass parts of the composition is, in particular, to 100 mass parts.

Determination of particle size lateralisation spectroscopy it is known from the literature and are described, for example, in T. Allen, Particle Size measurement, Bd.1, Kluver Academie Publishers, 1999.

The dispersant preferably includes at least one agent selected from the range: alkoxylate, alkylamide, ester, aminoxide, alkylpolyglucoside, ALKYLPHENOLS, arylalkylamine, water-soluble homopolymers, water-soluble random copolymers, water-soluble copolymers, water-soluble graft copolymers, particularly, polyvinyl alcohol, copolymers of polyvinyl alcohol and polyvinylacetate, polyvinylpyrrolidone, cellulose, starch, gelatin, gelatin derivatives, polymers of amino acids, polylysin, poliasparaginovaya acid, polyacrylates, polystyrenesulfonate, polystyrenesulfonate, polymethacrylate, condensation products of aromatic sulphonic acids with fomaldehyde, naphthalenesulfonate, lignosulfonates, copolymers of acrylic monomers, polyethylenimine, poly-vinylamine, polyallylamine, poly(2-vinylpyridine), blockcopolymer, blockcopolymer with polystyrene blocks and/or p is legallydownload.

Particularly preferably, the dispersant is selected from a range of: polyvinyl pyrrolidone, blockcopolymer, blockcopolymer with polystyrene blocks. Most preferably, use polyvinylpyrrolidone with a molecular weight of from about 8,000 of atomic mass units to 400,000 atomic mass (for example, PVP K15 - polyvinylpyrrolidone with a molecular weight of 10,000 atomic mass of the firm Fluka or PVP K90 (molecular weight of about 360000 of atomic mass units) of the company Fluka) and, most preferably, also blockcopolymer with polystyrene blocks with 62 wt.% C2-simple polyester, 23 wt.% C3-simple polyester and 15 wt.% polystyrene per dry disperser, with respect to the block length of C2-polyether to C3a simple polyester 7:2 units (for example, Disperbyk 190 firms BYK-Chemie, Wesel).

Solvent b), particularly preferably, choose from a number of: alcohols containing from 1 to 5 carbon atoms, in particular, alcohols containing from 1 to 3 carbon atoms, a simple ester, especially dioxolan, glycols, especially glycerol, ketones, especially acetone.

The foaming agent (d), preferably selected from the range: polydimethylsiloxane, polyacrylate, ammonium salts of polyacrylates, siloxanes, and combinations of waxes, copolymers with pigmentation groups, low molecular weight polymers, modified cellulose, especially hydroxic cellulose or methyl cellulose and carbon nanotube and polyvinyl alcohol, preferably, hydroxyethylcellulose, methylcellulose, and carbon nanotube. The preferred foaming agent (d) is selected from the group of the above-mentioned dispersant, and particularly preferably, for example dispersant BYK 356 firms BYK-Chemie, Wesel, polyacrylate, and BYK 154 of the same company, ammonium salt of acrylic copolymers. The foaming agent (d) may also be used in any combination, preferred is a combination of hydroxyethyl cellulose and/or methyl cellulose with carbon nanotubes.

Supplement e), preferably, choose from a number of: pigments, antifoam, light, optical bleaching agent, corrosion inhibitor, antioxidant, algicide, plasticizer, thickener, surface-active substances. Especially preferred is the addition of a reducing agent, such as formaldehyde, glycerin, ascorbic acid and so on, are particularly preferably used as an additive formaldehyde.

Conductive polymer f), preferably selected from a range of polypyrrol, polyaniline, polythiophene, polyphenylenevinylene, polyparaphenylene, polyethyleneoxide, polyfluorene, polyacetylene, most preferably, polyethyleneoxide in combination with polystyrenesulfonate. Conductive salt are preferably so-called ionage the nye liquid, especially salt type of tetraalkylammonium, pyridinium, imidazoline, tetraallylsilane with fluorinated anions.

Especially preferred composition is characterized by the fact that in it the silver particles (a) have an effective particle diameter of 10 to 150 nm, preferably from 20 to 80 nm, most preferably from 40 to 80 nm. Under the effective diameter of the particles of a mean average particle diameter, specific lateralisation spectroscopy (suitable device is, for example, Brookhaven BIC-90 Plus).

The silver particles (a)preferably contained in the composition in an amount of from 10 to 35 wt.h., most preferably 15 to 30 wt.h. The content of the dispersant (c)preferably ranges from 0.1 to 15 wt.h., most preferably from 5 to 10 wt.h.

Is also favorable if the particles in the finished composition to the same capable of forming a dense packing, leading already at low concentrations and temperatures of the processing to the desired conductivity of the filled structures. The requirement of low concentration due to purely economic reasons. The smaller may be supported by the content of particles with the same or similar to the conductivity, the lower the material cost of the resulting composition. When it is desired to replace as much as possible the mass number of particles on the natives substances.

In addition, the object of the invention is the use of a composition according to the invention to obtain a conductive coating, especially, conductive paths.

The object of the invention is also a method of obtaining a conductive tracks, characterized in that on the surface of the substrate put a new song in silk screen printing method, flexo, gravure or offset printing and thermoablative, especially at a temperature of not higher than 140°C, preferably not higher than 100°C to remove residual water and, if necessary, solvents, and, if necessary, for sintering contained particle of silver.

Especially preferred composition is characterized by the fact that it uses silver particles of various sizes. It was unexpectedly found that such a distribution of particle sizes is useful for the formation of conductive structures already at lower concentrations of silver nanoparticles. It is assumed that this is due to the filling of the formed intermediate volume between the larger particles to smaller particles. As a result, during subsequent thermal processing of the ink is increased arise continuous contact surface. So the resulting composition at a lower mass particle content achieves the same conductivity ink with almost monodisperse the first distribution of particles at nearly the same effective diameter of the particles or a higher conductivity for the same mass content and the same effective diameter of the particles.

The object of the invention is also a substrate, especially a transparent polymeric substrate having a conductive coating obtained from the composition according to the invention. Preferred is a substrate which has a conductive coating contains conductive paths with a conductivity of at least 5·105SIM/m

In addition, the above requirements are met by a composition comprising nanoparticles of silver, silver particles, a solvent, a foaming agent, a dispersant and additives. Preferably, it contains a small silver nanoparticles, which mainly have an effective diameter of from 20 to 80 nm, most preferably from 40 to 80 nm, with a bimodal distribution of particles in a concentration of from 5 to 40 wt.%, preferably, from 15 to 30 wt.%. The composition, for example, may be deposited on the polycarbonate, then dried and temperarure at a temperature of at least 80°C for several minutes. Then get very firmly fixed conductive patterns or, in the plane of the drawing, the optical reflective layers, in both cases, with high strength fastening on the polycarbonate.

Preferably used in the composition of the sols of silver obtained from the silver oxide recovery in such a reducing agent as an aqueous solution of formaldehyde is (FA) after prior addition of dispersant. This silver sols receive, for example, the rapid mixing of a solution of silver nitrate with sodium hydroxide by a strong high-speed mixer in a periodic process or in a continuous process using microsociety according to the still unpublished German patent application with the document number 102006017696. Directly after that nanoparticles of silver oxide restore an aqueous solution of formaldehyde (FA) in excess in a periodic way and then purified by centrifugation or membrane filtration, preferably, membrane filtration. This production method is particularly favorable when the number of bound on the surface of nanoparticles of organic auxiliary means supported at this small and, in addition, can be obtained bimodal distribution of particle sizes. In particular, it does require a pre-processing stage, such as pre-restoration in the presence of polymers, or additional stages of post-processing in addition to energy supply, such as, for example, the activating system of the preceding product or flocculation.

Example 1: (Getting silver nanoparticles).

0,054 molar silver nitrate solution was mixed with a mixture of 0,054 molar solution of sodium hydroxide and d is supergator Disperbyk 190 (manufacturer BYK Chemie) (1 g/l) in a volume ratio of 1:1 and stirred for 10 minutes. To this reaction mixture was added with stirring to 4.6 molar aqueous solution of formaldehyde, resulting in the ratio of silver ions Ag+the reducing agent was 1:10. This mixture was heated to 60°C, held at this temperature for 30 minutes and then cooled. The particles separated in the first stage, diafiltrate from unreacted components, and then the Sol was concentrated, for which we used a membrane with pore size of 30,000 daltons. Formed colloid-stable Sol with a solids content of 20 wt.% (silver particles and dispersant). The content of Disperbyk 190 after membrane filtration according to the elementary analysis was 6 wt.% based on the silver content. In the study method lateralisation spectroscopy (Brookhaven BIC-90 Plus) the effective particle diameter of 78 nm.

Example 2:

In 15 ml of 20%aqueous Sol of silver nanoparticles from Example 1 was dissolved 1.5 g of polyvinylpyrrolidone PVPK 40 (SIGMA-ALDRICH) and 1.5 g of dispersant Disperbyk 190 (Altana, Byk-Additives). Then the mixture is introduced 30 g of silver powder (Metolor K-1332 P) by means of ultrasound finger (G. Heinemann, Ultraschal und Labortechnik) with an amplitude of 30% of maximum power. Immediately after this, the paste is applied by screen printing on polycarbonate film (Makrolon®, Bayer MaterialScience AG) and temperatuur at 130°C. the Achieved conductivity 2·106/sup> SIM/m

1. The printed composition to obtain a conductive coating on the basis of the dispersed water particles of silver, containing at least:
a) from 5 to 40 wt.h. metallic silver particles with an effective diameter of 10 to 150 nm, a specific laser correlation spectroscopy, and the silver particles have a bimodal distribution of particle size;
b) from 50 to 99.5 wt.h. water and, if necessary, up to 30 wt.h. solvent;
c) from 0.01 to 15 wt.h., at least one dispersant;
d) from 0 to 5 wt.h. additives;
e) from 0 to 5 wt.h. conductive, optionally, water-soluble polymers,
characterized in that the composition additionally contains
f) from 0.5 to 5 wt.h. thickener and
g) from 30 to 70 wt.h. silver particles or copper particles, silver-plated with an effective diameter of from 500 nm to 10 μm,
and has a viscosity of at least 1 PA·S.

2. The composition according to p. 1, characterized in that the dispersant (c) is at least one agent selected from the range: alkoxylate, alkylolamides, esters, aminoxide, alkylpolyglucoside, ALKYLPHENOLS, arylalkylamine, water-soluble homopolymers, water-soluble random copolymers, water-soluble copolymers, water-soluble graft polymers, especially polyvinyl alcohols, copolymers of polyvinyl alcohols and polyvinyl is zlatov, polyvinylpyrrolidone, cellulose, starch, gelatin, gelatin derivatives, polymers of amino acids, polylysin, poliasparaginovaya acid, polyacrylates, polyarilensulphone, polystyrenesulfonate, polymethacrylates, condensation products of aromatic sulphonic acids with fomaldehyde, naphthalenesulfonate, ligninsulfonate, copolymers of acrylic monomers, polyethylenimine, polyvinylene, polyallylamine, poly(2-vinylpyridine), block-Capoliveri, blockcopolymer with polystyrene blocks and/or politically-dimethylammoniumchloride.

3. The composition according to p. 1, characterized in that the dispersant (c) is chosen from the range: blockcopolymer and blockcopolymer with polystyrene blocks.

4. The composition according to p. 1, wherein the other solvent (b) is chosen from the series: alcohols containing from 1 to 5 carbon atoms, in particular, alcohols containing from 1 to 3 carbon atoms, ethers, especially dioxolan, glycols, especially glycerol, ketones, especially acetone.

5. The composition according to p. 1, characterized in that the thickener f) is chosen from the series: polyacrylate, ammonium salts of polyacrylates, siloxanes, polyethylene glycol, combinations of waxes, low molecular weight polymers, modified cellulose, especially hydroxyethylcellulose or methylcellulose, carbon nanotube and polyvinyl alcohol, preferably hydroxyethylcellulose is for, methyl cellulose and carbon nanotube.

6. The composition according to p. 1, characterized in that the thickener f) is a mixture of hydroxyethyl cellulose and carbon nanotubes.

7. The composition according to p. 1, characterized in that the additive (d) is chosen from the series: pigments, defoamers, light stabilizers, optical brighteners, corrosion inhibitors, antioxidants, algaecides, plasticizers and thickeners, surface-active substances.

8. The composition according to p. 1, characterized in that the conductive polymer (e) is chosen from the series: polypyrrol, polyaniline, polythiophene, polyphenylenevinylene, polyparaphenylene, polyethyleneoxide, polyfluorene, polyacetylene, preferably polyethyleneoxide/polystyrenesulfonate.

9. The composition according to p. 1, characterized in that the content of silver particles (a) is from 10 to 35 wt.h., preferably from 15 to 30 wt.h.

10. Composition according to one of paragraphs.1-9, characterized in that the content of the dispersant (c) is from 0.1 to 15 wt.h., preferably from 5 to 10 wt.h.

11. The use of a composition according to one of paragraphs.1-10 to obtain a conductive coating.

12. The use of a composition according to p. 11, characterized in that elektroprovodnyi coatings are conductive paths.

13. A method of obtaining a conductive tracks, characterized in that the composition according to one of paragraphs.1-10 applied to p is the surface of the substrate by screen printing, flexo, gravure or offset printing and thermoablative at a temperature not exceeding 140°C to remove water and, optionally, a solvent.

14. A polymeric substrate having a conductive coating of the composition according to one of paragraphs.1-10.

15. The substrate under item 14, characterized in that the conductive coating contains conductive paths with a conductivity of at least 5·104SIM/M.



 

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21 cl, 5 tbl, 17 ex

FIELD: printing.

SUBSTANCE: invention relates to an ink set containing chromophoric metals for digital printing on ceramic materials. The ink set comprises liquid colouring compositions (A), (B), (C) and one from (D) and (E). The (A) comprises at least a compound of cobalt. The (B) comprises at least a compound of iron. The (C) comprises at least a compound of a metal selected from chromium, nickel and their mixtures. The (D) comprises at least a compound of cobalt and at least a compound of iron. The (E) comprises one or more compounds of zirconium. The said metal compounds decompose at a temperature of from 500 to 1300°C. When interacting with the ceramic material the metal compounds of compositions (A)-(D) form colured oxides or colured compounds. The compounds of zirconium from the composition (E) with the ceramic material form white oxides or white compounds. Also the method of decorating ceramic materials by digital printing using the specified set of ink and the decorated ceramic products produced using this method are described.

EFFECT: invention provides ceramic materials decorated with digital printing of wide range of colours with the effect of natural stone.

11 cl, 45 tbl, 5 ex

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