Ultra-bright passivated aluminum nano-flake pigments
View Patent ↗An organic release agent is vacuum deposited over a substrate and surface treated with a plasma or ion-beam source in a gas rich in oxygen-based functional groups to harden a very thin layer of the surface of the deposited layer in a passivating environment. Aluminum is subsequently vacuum deposited onto the hardened release layer to form a very flat and specular thin film. The film is exposed to a plasma gas containing oxygen or nitrogen to passivate its surface. The resulting product is separated from the substrate, crushed to brake up the film into aluminum flakes, and mixed in a solvent to separate the still extractable release layer from the aluminum flakes. The surface treatment of the release layer greatly reduces wrinkles in the flakes, improving the optical chracteristics of the flakes. The passivation of the flake material virtually eliminates subsequent corrosion from exposure to moisture.
1. A process for producing specular and passivated aluminum flakes in a vacuum chamber, comprising the following steps:
(a) flash-evaporating an organic material in the vacuum chamber to produce a vapor, said organic material being suitable for extraction by melting or dissolution;
(b) condensing the vapor over a substrate to produce an un-polymerized liquid layer of said organic material;
(c) exposing said liquid layer in vacuum to a first plasma source to produce cross-linking of a surface of said liquid layer of organic material, said cross-linking being substantially limited to only said surface so as not to affect the organic material's suitability for extraction by melting or dissolution, said first plasma source being operated with a first gas containing a first passivating component for aluminum;
(d) depositing aluminum in vacuum to form a film thereof on said cross-linked surface, said film containing a passivated aluminum surface produce by said first passivating component at an interface with the layer of organic material;
(e) exposing said film of aluminum to a second plasma source operated with a second gas containing a second passivating component for aluminum, such that a second passivated aluminum surface is produced by said second passivating component at a face of the film opposite said interface with the layer of organic material;
(f) crushing said film of aluminum; and
(g) extracting said organic material to produce aluminum flakes.
2. The process of claim 1 , wherein said first and second passivating components are selected from the group consisting of oxygen, nitrogen, and a mixture thereof.
3. The process of claim 1 , wherein said substrate is a rotating drum and said steps (a)-(e) are carried out continuously and repeatedly over the rotating drum.
4. The process of claim 1 , wherein said substrate is a web being spooled between two reels and said steps (a)-(e) are carried out continuously and repeatedly over the web.
5. The process of claim 1 , wherein said substrate is a web being spooled between two reels and said steps (a)-(e) are carried out continuously over the web alternately spooled in opposite directions between the two reels.
6. The process of claim 1 , wherein said organic material is selected from the group consisting of waxes, oligomers, and small organic molecules with molecular weight between 200 and 5,000.
7. The process of claim 1 , wherein said cross-linking of said surface of the liquid layer of organic material does not exceed 10 percent of the layer's thickness.
8. The process of claim 1 , further including the step of mixing the aluminum flakes with a binder to produce a specular reflective pigment.
9. The process of claim 1 , further including the step of using an optical densitometer to control a thickness of said film of aluminum.
10. The process of claim 1 , wherein said steps (a) and (b) are carried out at a pressure less than about 1 torr; said steps (c) and (e) are carried out at a pressure between approximately 10 −1 and 10 −3 torr; and said step (d) is carried out at a pressure less than about 10 −4 torr.
11. The process of claim 1 , further including the step of treating said substrate with a plasma source prior to said step (a).
12. The process of claim 1 , wherein said first and second gases are the same.
13. A process for producing metallic flakes in a vacuum chamber, comprising the following steps:
(a) flash-evaporating an organic material in the vacuum chamber to produce a vapor, said organic material being suitable for extraction by melting or dissolution;
(b) condensing the vapor over a substrate to produce an un-polymerized layer of said organic material;
(c) exposing said liquid layer in vacuum to a plasma source to produce cross-linking of a surface of said liquid layer of organic material, said cross-linking being substantially limited to only said surface so as not to affect the organic material's suitability for extraction by melting or dissolution;
(d) depositing a metallic flake material in vacuum to form a film thereof on said layer of organic material;
(e) crushing said film of metallic flake material; and
(f) extracting said organic material to produce metallic flakes.
14. The process of claim 13 , wherein said substrate is a rotating drum and said steps (a)-(d) are carried out continuously over the rotating drum.
15. The process of claim 13 , wherein said substrate is a web being spooled between two reels and said steps (a)-(d) are carried out continuously over the web.
16. The process of claim 13 , wherein said substrate is a web being spooled between two reels and said steps (a)-(d) are carried out continuously over the web alternately spooled in opposite directions between the two reels.
17. The process of claim 13 , wherein said metallic flake material is selected from the group consisting of metal oxides, gold, silver, palladium, platinum, chromium, nickel, indium and copper.
18. The process of claim 13 , wherein said organic material is selected from the group consisting of waxes, oligomers, and small organic molecules with molecular weight between 200 and 5,000.
19. The process of claim 13 , wherein said organic material is a monofunctional monomer, and the process further includes the step of curing the layer of organic material prior to said step (c).
20. The process of claim 13 , wherein said cross-linked surface in said layer of organic material does not exceed 10 percent of the layer's thickness.
21. The process of claim 13 , wherein said metallic flake materials selected from the group consisting of aluminum, silver, chromium, nickel, indium, and copper; and the process further includes a step of operating said surface treatment source with a gas containing a passivating component.
22. The process of claim 13 , wherein said metallic flake material is selected from the group consisting of ITO and IZO; and the process further includes a step of operating said surface treatment source with a gas containing oxygen.