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1. WO2013128449 - ENCRES CONTENANT DES NANOPARTICULES PRÉCURSEURS MÉTALLIQUES

Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique

[ EN ]

CLAIMS:

1. A printing formulation (ink) comprising at least one metal precursor selected from:

(1) metal precursor in the form of metal salt nanoparticles dispersed in a medium, and

(2) metal precursor in the form of a metal complex dissolved in a medium, wherein said complex having one or more hydroxy amine or aminoacid complexing moieties.

2. The printing formulation of claim 1, further comprising at least one printing suitable liquid carrier.

3. A printing formulation (ink) comprising at least one printing suitable liquid carrier and at least one metal precursor selected from:

(1) metal precursor in the form of metal salt nanoparticles dispersed in a medium, and

(2) metal precursor in the form of a metal complex dissolved in a medium, wherein said complex having one or more hydroxy amine or amino acid complexing moieties.

4. The printing formulation according to claim 1, comprising at least one metal precursor in the form of metal salt nanoparticles dispersed in a medium.

5. The printing formulation of any one of the preceding claims, wherein the mean particle size of the metal salt nanoparticles is between about 10 nm and 1,000 nm.

6. The printing formulation of claim 5, wherein the mean particle size of the metal salt nanoparticles is between about 50 nm and 1,000 nm.

7. The printing formulation of any one of claims 1 to 6, wherein the metal salt nanoparticles have random shapes, or are substantially spherical or are crystalline or amorphous.

8. The printing formulation of any one of claims 1 to 7, wherein the nanoparticulate metal salt is obtained by a process selected from bead milling, spray drying and precipitation.

9. The printing formulation of claim 8, wherein the nanoparticulate metal salt is obtained by bead milling.

10. The printing formulation of claim 9, wherein bead milling involves milling a mixture of the metal salt, a stabilizer and a solvent at the presence of beads.

11. The printing formulation of claim 8, wherein the nanoparticulate metal salt precursor is obtained by precipitation, by adding a precipitation agent to a solution of a precursor material.

12. The printing formulation of claim 11 , wherein said precipitation is carried out in the presence of a stabilizer.

13. The printing formulation of any one of claims 1 to 12, wherein said metal precursor is of a metal of Groups IIIB, IVB, VB, VIB, VIIB, VIIIB, IB and IIB of block d of the Periodic Table of Elements.

14. The printing formulation of claim 13, wherein said metal is selected from Sc, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Y, Zr, Nb, Tc, Ru, Mo, Rh, W, Au, Pt, Pd, Ag, Mn, Co, Cd, Hf, Ta, Re, Os, Al, Sn, In, Ga and Ir.

15. The printing formulation of claim 14, wherein said metal is selected from Cu, Ni, Ag, Au, Pt, Pd, Al, Fe, Co, Ti, Zn, In, Sn and Ga.

16. The printing formulation of claim 15, wherein said metal is selected from Cu, Ni and Ag.

17. The printing formulation of claim 15, wherein said metal is selected from Cu and Ni.

18. The printing formulation of claim 15, wherein said metal is Cu.

19. The printing formulation of any one of claims 1 to 18, wherein said metal salt comprises an inorganic anion or an organic anion.

20. The printing formulation of claim 19, wherein said inorganic anion is selected from HO", F~, CF, Br", Γ, N02", N03~, C104~, S04"2, S03", P04" and C03"2.

21. The printing formulation of claim 19, wherein said organic anion is selected from acetate (CH3COO~), formate (HCOCT), citrate (C3H50(COO)3~3), acetylacetonate, lactate (CH3CH(OH)COO"), oxalate ((COO)2~2), and any derivative thereof.

22. The printing formulation of claim 1 , wherein the metal salt is salt of copper.

23. The printing formulation of claim 22, wherein the copper metal salt is selected from copper formate, copper citrate, copper acetate, copper nitrate, copper acetylacetonate, copper perchlorate, copper chloride, copper sulfate, copper carbonate, copper hydroxide and mixtures thereof.

24. The printing formulation of claim 1 , wherein the metal salt is a salt of nickel.

25. The printing formulation of claim 24, wherein the nickel metal salt is selected from nickel formate, nickel citrate, nickel acetate, nickel nitrate, nickel acetylacetonate, nickel perchlorate, nickel chloride, nickel sulfate, nickel carbonate, nickel hydroxide and mixtures thereof.

26. The printing formulation of claim 1 , wherein the metal salt is a salt of silver.

27. The printing formulation of claim 26, wherein the silver metal salt is selected from silver oxalate, silver lactate, silver formate and mixtures thereof.

28. The printing formulation of claim 1 , wherein the metal salt is selected from indium(III) acetate, indium(III) chloride, indium(III) nitrate; iron(II) chloride, iron(III) chloride, iron(II) acetate; gallium(III) acetylacetonate, gallium(II) chloride, gallium(III) chloride, gallium(III) nitrate; aluminum(III) chloride, aluminum(III) stearate; silver nitrate, silver chloride; dimethlyzinc, diethylzinc, zinc chloride, tin(II) chloride, tin(IV) chloride, tin(II) acetylacetonate, tin(II) acetate; lead(II) acetate, lead(II) acetlylacetonate, lead(II) chloride, lead(II) nitrate and PbS.

29. The printing formulation of any one of claims 1 to 28, wherein the nanoparticulate metal salt material is formulated as dispersion in a liquid medium.

30. The printing formulation of claim 29, wherein said liquid medium is water or a water-containing liquid mixture.

31. The printing formulation of claim 29, wherein said liquid medium is an organic solvent.

32. The printing formulation of claim 29, wherein said liquid medium is a water-containing organic solvent.

33. The printing formulation of claim 31, wherein said organic solvent is selected from glycol ether, alcohol and acetate.

34. The printing formulation of claim 33, wherein said organic solvent is selected from terpinol, acetone, ethyl acetate, ethanol, propanol, butanol, and combinations thereof.

35. The printing formulation of any one of claims 29 to 34, wherein the dispersion further comprises a stabilizing agent.

36. The printing formulation of claim 35, wherein the stabilizing agent is selected from the liquid medium, a polyelectrolyte, a polymeric material, a cationic surfactant, an anionic surfactant, a non-ionic surfactant, a zwitterionic surfactant and a cationic polymer.

37. The printing formulation of claim 1, wherein said metal precursor being metal salt nanoparticles of copper formate dispersed in glycol ether, and further comprising a stabilizer being a functionalized polymer.

38. The printing formulation of claim 37, wherein the stabilizing agent is a copolymer or salt of a copolymer having acidic groups.

39. The printing formulation of any one of claims 1 to 38, further comprising an additive selected from humectants, binders, surfactants, fungicides, rheology modifiers, pH adjusting agents, wetting agents, adhesion promoter and mixtures thereof.

40. The printing formulation of claim 1, comprising at least one metal precursor in from of a metal complex in a liquid medium.

41. The printing formulation of claim 40, wherein the metal complex comprises organic complexing moieties.

42. The printing formulation of claim 41, wherein said complexing moieties are amino acids.

43. The printing formulation of claim 41, wherein the metallic complex is selected from a copper complex, a nickel complex, an aluminum complex, a cobalt complex, a tin complex, an indium complex, and a zinc complex.

44. The printing formulation of claim 43, wherein the metal is copper and the copper complex is selected to easily decompose at a low temperature.

45. The printing formulation of claim 43, wherein the copper complex comprises amine and hydroxy complexing moieties.

46. The printing formulation of claim 45, wherein the complexing moieties are selected from ethanol amine, di-ethanol amine, triethanol amine, amino methyl propanol (AMP 95), l-amino-2-propanol, 3 -amino- 1 -propanol and diisopropanolamine.

47. The printing formulation of any one of claims 40 to 46, wherein the medium in which the metal complexes are dissolved is water or a water-containing liquid mixture.

48. The printing formulation of any one of claims 40 to 46, wherein the medium in which the metal complexes are dissolved is an organic solvent.

49. The printing medium of claim 48, wherein said organic solvent is selected from glycol ether, alcohol and acetate.

50. The printing formulation of claim 49, wherein said organic solvent is selected from terpinol, acetone, ethyl acetate, ethanol, propanol, butanol, and combinations thereof.

51. The printing formulation of any one of claims 40 to 50, further comprising an additive selected from humectants, binders, surfactants, fungicides, rheology modifiers, pH adjusting agents, adhesion promoter, wetting agent and mixtures thereof.

52. A printing formulation of any one of claims 1 to 51, for use in coating a substrate surface.

53. The printing formulation of claim 52, wherein said coating is carried out by a method selected from spin coating, roll coating, spray coating, dip coating, flow coating, doctor blade coating, dispensing, ink-jet printing, offset printing, screen printing, pad printing, gravure printing, flexography, nanoimprinting, stencil printing, imprinting, xerography, lithography and stamping.

54. A printing formulation of any one of claims 1 to 51, for use in the production of EMI shielding materials, conductive adhesives, low-resistance metal wirings, PCBs, FPCs, antennas for RFID tags, solar cells, secondary cells or fuel cells, electrodes or wiring materials for TFT-LCDs, OLEDs, flexible displays, OTFTs, and sensors.

55. An ink formulation comprising a printing formulation of any one of claims 1 to 54.

56. The ink formulation of claim 55, being in a liquid form, or a solid form.

57. A method of forming a printing formulation, the method comprising:

-obtaining a metal precursor selected from

(1) metal precursor in a form of metal salt nanoparticles; and

(2) metal precursor in a form of a metal complex,

wherein:

-when the metal precursor is nanoparticles of a metal salt, dispersing the nanoparticles in a liquid medium, or

-when the metal precursor is a metal complex, dissolving the metal complex in a liquid medium.

58. The method according to claim 57, wherein said metal precursor being in the form of metal salt nanoparticles, and the method comprising dispersing the nanoparticles in a liquid medium.

59. The method according to claim 57, wherein said metal precursor being in the form of a metal complex, and the method comprising dissolving the metal complex in a liquid medium.

60. A process for forming a conductive pattern on a surface region of a substrate, the process comprising:

obtaining a substrate;

on at least a surface region of a substrate forming a pattern of a printing formulation according to any one of claims 1 to 55, the formulation comprising at least one metal precursor selected from:

(1) metal precursor in the form of metal salt nanoparticles dispersed in a medium (as detailed hereinabove); and

(2) metal precursor in the form of a metal complex dissolved in a medium;

decomposing said metal precursor in said pattern to obtain a metallic pattern.

61. The process of claim 60, further comprising the step of sintering the metallic pattern.

62. The process of claim 60 or 61, wherein said step of decomposing is achievable by heating, heating in an oven, heating by laser, heating by microwave, heating by electrical voltage, or heating by exposure to light.

63. The process of claim 60 or 61, wherein said step of decomposing is achievable by photonic curing by UV radiation, IR radiation or by plasma treatment.

64. The process of claim 62, wherein said decomposing is achievable by heating under air, nitrogen, argon or a non-oxidizing atmosphere.

65. The process of claim 60 or 61, wherein said decomposing is achievable by heating under air or an oxidizing atmosphere.

66. The process of claim 60 or 61, wherein said decomposing is achievable by a chemical method.

67. The process of any one of claims 57 to 66, wherein said substrate is a flexible substrate or a rigid substrate.

68. The process of claim 67, wherein said substrate is selected from a plastic substrate, a glass substrate, a metallic substrate, a silicon substrate, a germanium substrate, an ITO substrate, an FTO substrate, and a T1O2 substrate.

69. A conductive pattern obtainable by the process of any one of claims 60 to 68.

70. An element comprising a conductive pattern, wherein said conductive pattern comprises a metallic material being substantially free of metal oxide at the time of manufacture.

71. The element of claim 70, wherein said conductive pattern obtainable by the process of any one of claims 60 to 68.

72. An element comprising a conductive pattern, wherein said conductive pattern having high oxidation resistance at ambient atmosphere.

73. The element of claim 72, wherein said conductive pattern obtainable by the process of any one of claims 60 to 68.

74. A printing formulation according to claim 1, comprising at least one metal complex, wherein the at least one metal atom being associated to at least two different organic moieties.

75. A printing formulation according to claim 1, comprising at least one metal complex, wherein the at least one metal atom being associated to at least one additive.

76. The printing formulation of claim 75, wherein the additive is selected from conducting metallic particles, conducting metallic nanoparticles, a metal precursor, an oxidant, an anti-oxidant, a stabilizer, a solvent, a humectant, a dispersing agent, a binder, a reducing agent, a surfactant, a wetting agent and a leveling agent.

77. A printing formulation (ink) comprising a medium and a combination of:

(1) metal precursor in the form of metal salt nanoparticles dispersed in said medium; and

(2) metal precursor in the form of a metal complex dissolved in said medium.