CA2634457A1 - Synthesis of metallic nanoparticle dispersions - Google Patents

Synthesis of metallic nanoparticle dispersions Download PDF

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Publication number
CA2634457A1
CA2634457A1 CA002634457A CA2634457A CA2634457A1 CA 2634457 A1 CA2634457 A1 CA 2634457A1 CA 002634457 A CA002634457 A CA 002634457A CA 2634457 A CA2634457 A CA 2634457A CA 2634457 A1 CA2634457 A1 CA 2634457A1
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CA
Canada
Prior art keywords
oxide
composition
range
metallic
nanoparticles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002634457A
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French (fr)
Inventor
Gregory A. Jablonski
Michael A. Mastropietro
Christopher J. Wargo
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
PChem Associates Inc
Original Assignee
Pchem Associates, Inc.
Gregory A. Jablonski
Michael A. Mastropietro
Christopher J. Wargo
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Filing date
Publication date
Application filed by Pchem Associates, Inc., Gregory A. Jablonski, Michael A. Mastropietro, Christopher J. Wargo filed Critical Pchem Associates, Inc.
Publication of CA2634457A1 publication Critical patent/CA2634457A1/en
Abandoned legal-status Critical Current

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Classifications

    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • 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

Abstract

Disclosed are compositions comprising metallic nanoparticles suitable for use in cohesive, highly conductive structures on substrates. Also disclosed are methods for synthesizing the compositions and methods for forming cohesive, highly conductive structures from the compositions.

Claims (105)

1. A composition, comprising:

a population of metallic nanoparticles dispersed in an aqueous medium, wherein at least a portion of the population comprising individual metallic nanoparticles characterized as having an average cross-sectional dimension in the range of from about 1 nm to about 100 nm; and, wherein each of the nanoparticles comprise at least one ligand bound to its surface, the ligand comprising a heteroatom head group bound to the nanoparticle surface and a tail bound to the heteroatom head group.
2. The composition of claim 1, wherein the nanoparticle population further comprises particle agglomerate comprised of two or more individual nanoparticles, nanoparticle floc comprised of two or more individual nanoparticles, or any combination thereof.
3. The composition of claim 2, wherein the ratio, by weight, of the population of individual metallic nanoparticles to particle agglomerate is in the range of from about 1:99 to 99:1.
4. The composition of claim 2, wherein the ratio, by weight, of the population of individual metallic nanoparticles to particle floc is in the range of from about 1:99 to 99:1.
5. The composition of claim 2, a nanoparticle agglomerate has an average cross-sectional dimension in the range of from about 100 nm to about 10000 nm.
6. The composition of claim 2, wherein a nanoparticle floc has an average cross-sectional dimension in the range of from about 100 to about 10000 nm.
7. The composition of claim 1, wherein an individual metallic nanoparticle comprises silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, silver oxide, copper oxide, gold oxide, zinc oxide, cadmium oxide, palladium oxide, iridium oxide, ruthenium oxide, osmium oxide, rhodium oxide, platinum oxide, iron oxide, nickel oxide, cobalt oxide, indium oxide, or any combination thereof.
8. The composition of claim 1, wherein the aqueous medium is capable of solvating the metallic salt in a range of from about 10 grams/liter to about 600 grams/liter.
9. The composition of claim 1, wherein the nanoparticles are present in the range of from about 0.5 wt % to about 70 wt %.
10. The composition of claim 1, wherein the ligand is present in the range of from about 0.5 wt % to about 75 wt %.
11. The composition of claim 1, wherein the medium is present in the range of from about 30 to about 98 wt %.
12. The composition of claim 1, wherein the composition is capable of forming a cohesive structure of less than about 10 µm in thickness following curing at a temperature of less than about 140°C for less than about 60 seconds.
13. The composition of claim 12, wherein the structure has a resistivity in the range of from about 2 times to about 15 times the bulk resistivity of the corresponding metal.
14. A composition, comprising:

a metallic nanoparticle mixture comprising at least one metallic nanoparticles, capable of forming a cohesive structure of less than about 10 µm in thickness following curing at a temperature of less than about 140°C for less than about 90 seconds, wherein the cohesive structure has a resistivity in the range of from about 2 times to about 15 times the bulk resistivity of the corresponding metal.
15. The composition of claim 14, wherein the mixture comprises a population of metallic nanoparticles, a ligand, an aqueous medium, or any combination thereof.
16. The composition of claim 15, wherein the nanoparticle population comprises individual nanoparticles, particle agglomerate comprised of two or more individual nanoparticles, particle floc comprised of two or more individual nanoparticles, or any combination thereof.
17. The composition of claim 16, wherein the ratio, by weight, of the population of individual metallic nanoparticles to particle agglomerate is in the range of from about 1:99 to 99:1.
18. The composition of claim 16, wherein the ratio, by weight, of the population of individual metallic nanoparticles to particle floc is in the range of from about 1:99 to 99:1.
19. The composition of claim 16, wherein individual metallic nanoparticles have an average cross-sectional dimension in the range of from about 1 nm to about 100 nm.
20. The composition of claim 16, wherein particle agglomerates have an average cross-sectional dimension in the range of from about 100 nm to about 10000 nm.
21. The composition of claim 16, wherein particle flocs have an average cross-sectional dimension in the range of from about 100 to about 10000 nm.
22. The composition of claim 16, wherein an individual metallic nanoparticle comprises silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, silver oxide, copper oxide, gold oxide, zinc oxide, cadmium oxide, palladium oxide, iridium oxide, ruthenium oxide, osmium oxide, rhodium oxide, platinum oxide, iron oxide, nickel oxide, cobalt oxide, indium oxide, or any combination thereof.
23. The composition of claim 15, wherein the aqueous medium is capable of solvating the metallic salt in a range of from about 10 grams/liter to about 600 grams/liter.
24. The composition of claim 15, wherein the nanoparticles are present in the range of from about 0.5 to about 70 wt %.
25. The composition of claim 15, wherein the ligand is present in the range of from about 0.5 to about 75 wt %.
26. The composition of claim 15, wherein the medium is present in the range of from about 30 to about 98 wt %.
27. A method for synthesizing a metallic nanoparticle dispersion, comprising:
reacting in an aqueous medium:

at least one ligand, wherein the ligand comprises a heteroatom head group bonded to a tail comprising from 1 to about 20 carbon atoms;

at least one reducing agent; and, at least one metallic salt in an aqueous dispersing solution, wherein the metallic salt is present in the dispersion at a concentration in the range of from about 10 grams/liter to about 600 grams/liter based on volume of the dispersing solution, and wherein the metallic salt comprises at least one cation comprising silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, or any combination thereof.
28. The method of claim 27, wherein the ligand is characterized as being capable of binding by its heteroatom head group to a surface of a metallic nanoparticle so as to give rise to a metallic nanoparticle stabilized at least in part against aggregation.
29. The method of claim 27, wherein the metallic salt further comprises at least one anion.
30. The method of claim 27, wherein the reacting comprises contacting, mixing, stirring, sonicating, agitating, or any combination thereof.
31. The method of claim 30, wherein, after the reacting, one or more ligand heteratomic head groups are characterized as bound to a surface of one or more metallic nanoparticles so as to give rise to one or more metallic nanoparticles stabilized against irreversible aggregation.
32. The method of claim 30, wherein the method further comprises combining the ligand and metallic salt in a respective molar ratio in the range of from about 0.1:1 to about 1:1.
33. The method of claim 32, wherein the method further comprises combining the metallic salt and reducing agent in a respective molar ratio in the range of from about 1:10 to about 4:1.
34. The method of claim 32, wherein the method further comprises adjusting the relative amounts of ligand, reducing agent, metallic salt, aqueous dispersing solution, adjusting the pH of the aqueous medium, or any combination thereof, so as to give rise to a pH in the range of from about 3 to about 12.
35. The method of claim 27 wherein the method further comprises heating the aqueous medium, ligand, reducing agent, and metallic salt in aqueous dispersing solution, or any combination thereof, to a temperature of from about 5 C to about 200 C prior to reaction.
36. The method of claim 27, wherein the method further comprises heating the aqueous medium, ligand, reducing agent, and metallic salt in aqueous dispersing solution, or any combination thereof, to a temperature of from about 35 C to about 70 C prior to reaction.
37. The method of claim 27, wherein the method further comprises heating the aqueous medium, ligand, reducing agent, and metallic salt in aqueous dispersing solution, or any combination thereof, to a temperature of from about 40 C to about 60 C prior to reaction.
38. The method of claim 27, further comprising a recovery step following reaction.
39. The method of claim 38, wherein the recovery step comprises allowing the passage of sufficient time such that the concentration of nanoparticles in any aqueous medium present is in the range of from about 0 wt % to about 70 wt%.
40. The method of claim 38, wherein the recovery step comprises allowing the passage of sufficient time such that the concentration of nanoparticles in any aqueous medium present is about 5 wt% and decanting the aqueous medium.
41. The method of claim 27, wherein the reacting comprises continuously introducing the aqueous medium, ligand, and reducing agent into a first stirred reactor capable of fluid communication with the contents of a second stirred reactor.
42. The method of claim 41, wherein the ligand is characterized as being capable of binding by its heteroatom head group to a surface of a metallic nanoparticle so as to give rise to a metallic nanoparticle stabilized at least in part against irreversible aggregation.
43. The method of claim 41, further comprising continuously introducing the metallic salt dispersion to the first reactor.
44. The method of claim 43, wherein the metallic salt further comprises an anion.
45. The method of Claim 44, wherein the anion comprises acetate, nitrate, carboxylate, sulfate, chloride, hydroxide, or any combination thereof.
46. The method of claim 43, wherein the dispersing medium comprises an aqueous medium substantially free of organic solvents.
47. The method of claim 44, wherein the ligand and metallic salt are introduced to the first reactor at a respective molar ratio of from about 0.1:1 to about 1:1.
48. The method of claim 43, further comprising adjusting the relative amounts of ligand, reducing agent, metallic salt, aqueous dispersing solution, adjusting the pH of the aqueous medium, or any combination thereof, so as to give rise to a pH in the range of from about 3 to about 12.
49. The method of claim 48, wherein the method further comprises heating the aqueous medium, ligand, reducing agent, and metallic salt in aqueous dispersing solution, or any combination thereof, to a temperature of from about 5°C to about 200°C before reaction.
50. The method of claim 43, wherein the method further comprises heating the aqueous medium, ligand, reducing agent, and metallic salt in aqueous dispersing solution, or any combination thereof, to a temperature of from about 35°C to about 70°C before reaction.
51. The method of claim 43, wherein the method further comprises heating the aqueous medium, ligand, reducing agent, and metallic salt in aqueous dispersing solution, or any combination thereof, to a temperature of from about 40°C to about 60°C before reaction.
52. The method of claim 43, wherein the residence time of the first reactor is sufficient so as to give rise to the reaction progressing to substantial completion.
53. The method of claim 43, further comprising continuously transporting the contents of the first reactor to the second reactor.
54. The method of claim 53, wherein the residence time in the second reactor is sufficient to allow the reaction to progress to essentially total completion.
55. The method of claim 54, further comprising a recovery step following reaction.
56. The method of claim 55, wherein the recovery step comprises allowing the passage of sufficient time such that the concentration of nanoparticles in any aqueous medium present is about 5 wt%.
57. A method for forming a conductive structure on a substrate, comprising:
depositing a composition onto the substrate, wherein the composition comprises at least one population of metallic nanoparticles, wherein at least a portion of the population comprising individual metallic nanoparticles characterized as having an average cross-sectional dimension in the range of from about 1 nm to about nm;

wherein each of the nanoparticles comprise at least one ligand bound to its surface, the ligand comprising a heteroatom head group bound to the nanoparticle surface and a tail bound to the heteroatom head group; and, curing the deposited composition.
58. The method of claim 57, wherein depositing comprises a printing method.
59. The method of claim 58, wherein the printing method comprises flexographic printing, rotogravure printing, lithographic printing, intaglio printing, relief printing, screen printing, inkjet printing, laser printing, or any combination thereof.
60. The method of claim 57, wherein the nanoparticle population comprises individual particles, nanoparticle agglomerate comprised of at least two individual nanoparticles, nanoparticle floc comprised of at least two nanoparticles, or any combination thereof.
61. The method of claim 57, wherein an individual metallic nanoparticle comprises silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, silver oxide, copper oxide, gold oxide, zinc oxide, cadmium oxide, palladium oxide, iridium oxide, ruthenium oxide, osmium oxide, rhodium oxide, platinum oxide,, iron oxide, nickel oxide, cobalt oxide, indium oxide, or any combination thereof.
62. The method of claim 57, wherein one or more ligands are characterized as bound to a surface of one or more metallic nanoparticles so as to give rise to one or more metallic nanoparticles stabilized against aggregation.
63. The method of claim 57, wherein the nanoparticles are present in the range of from about 0.5 to about 70 wt %.
64. The method of claim 57, wherein the ligand is present in the range of from about 0.5 to about 75 wt %.
65. The method of claim 57, wherein the composition further comprises a rheology modifier.
66. The method of claim 65, wherein the rheology modifier comprises an associative thickener.
67. The method of claim 65, wherein the rheology modifier comprises a thickening agent.
68. The method of claim 67, wherein the thickening agent comprises an alkali-soluble emulsion.
69. The method of claim 65, wherein the rheology modifier is present in the range of from about 0 wt% to about 15 wt%.
70. The method of claim 57, wherein the composition further comprises a binder.
71. The method of claim 70, wherein the binder is present in the range of from about 0 wt% to about 20 wt%.
72 The method of claim 57, wherein the substrate comprises a glass, a ceramic, a polymer, a silicon, a nitride, a carbide, a ceramic precursor, fabric, or any combination thereof.
73. The method of claim 72, wherein the polymer comprises a polyester, a polyolefin, a polycarbonate, an acrylic polymer, polyethylene naphthalate, polyimide, polyamideimide, polyvinyl chloride, polypropylene, a liquid crystal polymer, polycarbonate, or any combination thereof.
74. The method of claim 72, wherein the substrate further comprises paper, synthetic engineered paper, cardboard, a coated corrugated cardboard, an uncoated corrugated cardboard, or any combination thereof.
75. The method of claim 72, wherein at least a portion of a surface of the substrate is capable of being modified to give rise to a surface capable of adhering to the deposited composition.
76. The method of claim 57, wherein the composition further comprises metallic particles.
77. The method of claim 76, wherein the metallic particles have a width in the range of from about 200 nm to about 20000 nm.
78. The method of claim 76, wherein a metallic particle comprises silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, silver oxide, copper oxide, gold oxide, zinc oxide, cadmium oxide, palladium oxide, iridium oxide, ruthenium oxide, osmium oxide, rhodium oxide, platinum oxide, iron oxide, nickel oxide, cobalt oxide, indium oxide, or any combination thereof.
79. The method of claim 57, wherein curing comprises exposing the deposited composition to a temperature of less than about 140°C for less than about 90 seconds.
80. The method of claim 57, wherein the structure has a thickness of less than about 20 µm.
81. A method for forming a conductive structure, comprising:

depositing a metallic nanoparticle composition comprising at least one metallic nanoparticle onto the substrate, wherein the composition is capable of forming after curing at a temperature of less than about 140°C for less than about 90 seconds a cohesive and conductive structure having a resistivity in the range of from about 2 times to about 15 times the bulk resistivity of the corresponding metal and having a thickness of less than about 20 µm; and, curing the deposited composition.
82 The method of claim 81, wherein depositing comprises a printing method.
83. The method of claim 82, wherein the printing method comprises flexographic printing, rotogravure printing, lithographic printing, intaglio printing, relief printing, screen printing, inkjet printing, laser printing, or any combination thereof.
84. The method of claim 81, wherein the composition comprises a population of metallic nanoparticles, a ligand, a medium, or any combination thereof.
85. The method of claim 81, wherein the nanoparticle population comprises individual nanoparticles, nanoparticle agglomerate, nanoparticle floc, or any combination thereof.
86. The method of claim 85, wherein individual metallic nanoparticles have an average cross-sectional dimension in the range of from about 1 nm to about 100 nm.
87. The method of claim 85, wherein nanoparticle flocs have an average cross-sectional dimension in the range of from about 100 to about 10000 nm.
88. The method of claim 84, wherein an individual metallic nanoparticle comprises silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, silver oxide, copper oxide, gold oxide, zinc oxide, cadmium oxide, palladium oxide, iridium oxide, ruthenium oxide, osmium oxide, rhodium oxide, platinum oxide, iron oxide, nickel oxide, cobalt oxide, indium oxide, or any combination thereof.
89. The method of claim 84, wherein one or more ligands are characterized as bound to a surface of one or more metallic nanoparticles so as to give rise to one or more metallic nanoparticles stabilized against irreversible aggregation.
90. The method of claim 84, wherein the nanoparticles are present in the range of from about 0.5 to about 70 wt %.
91. The method of claim 84, wherein the ligand is present in the range of from about 0.5 to about 75 wt %.
92. The method of claim 84, wherein the medium is present in the range of from about 30 to about 98 wt %.
93. The method of claim 84, wherein the composition further comprises a rheology modifier.
94. The method of claim 93, wherein the rheology modifier comprises an associative thickener.
95. The method of claim 93, wherein the rheology modifier is present in the range of from about 0 wt% to about 15 wt%.
96. The method of claim 84, wherein the composition further comprises a binder.
97. The method of claim 96, wherein the binder comprises a latex, a polymer latex, an emulsion polymer, polyimide, a silicone, a fluorocarbon, a polyamic acid, a polyurethane, a polyester, an epoxy, or any combination thereof.
98. The method of claim 96, wherein the binder is present in the range of from about 0 wt% to about 20 wt%.
99. The method of claim 81, wherein the substrate comprises a glass, a ceramic, a polymer, a silicon, a nitride, a carbide, a ceramic precursor, fabric, or any combination thereof.
100. The method of claim 99, wherein the polymer comprises a polyester, a polyolefin, a polycarbonate, an acrylic polymer, polyethylene naphthalate, polyimide, polyamideimide, polyvinyl chloride, polypropylene, a liquid crystal polymer, polycarbonate, or any combination thereof.
101. The method of claim 99, substrate further comprises paper, synthetic engineered paper, cardboard, a coated corrugated cardboard, an uncoated corrugated cardboard, or any combination thereof.
102. The method of claim 99, wherein at least a portion of a surface of the substrate is capable of being modified to give rise to a surface capable of adhering to the deposited composition.
103. The method of claim 84, wherein the composition further comprises metallic particles.
104. The method of claim 103, wherein the metallic particles have a width in the range of from about 200 nm to about 20000 nm.
105. The method of claim 103, wherein a metallic particle comprises silver, copper, gold, zinc, cadmium, palladium, iridium, ruthenium, osmium, rhodium, platinum, iron, nickel, cobalt, indium, silver oxide, copper oxide, gold oxide, zinc oxide, cadmium oxide, palladium oxide, iridium oxide, ruthenium oxide, osmium oxide, rhodium oxide, platinum oxide, iron oxide, nickel oxide, cobalt oxide, indium oxide, or any combination thereof.
CA002634457A 2005-12-20 2006-12-20 Synthesis of metallic nanoparticle dispersions Abandoned CA2634457A1 (en)

Applications Claiming Priority (9)

Application Number Priority Date Filing Date Title
US75214405P 2005-12-20 2005-12-20
US75214305P 2005-12-20 2005-12-20
US60/752,144 2005-12-20
US60/752,143 2005-12-20
US75262805P 2005-12-21 2005-12-21
US60/752,628 2005-12-21
US11/613,136 2006-12-19
US11/613,136 US20070144305A1 (en) 2005-12-20 2006-12-19 Synthesis of Metallic Nanoparticle Dispersions
PCT/US2006/048699 WO2008048316A2 (en) 2005-12-20 2006-12-20 Synthesis of metallic nanoparticle dispersions

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CA2634457A1 true CA2634457A1 (en) 2008-04-24

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US (1) US20070144305A1 (en)
EP (1) EP1973682A4 (en)
JP (2) JP5394749B2 (en)
AU (1) AU2006350054B2 (en)
CA (1) CA2634457A1 (en)
WO (1) WO2008048316A2 (en)

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