Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
  • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
  • C23C16/40—Oxides
  • C23C16/406—Oxides of iron group metals
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
  • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges

Definitions

• the present invention provides a method for forming nano-structured iron oxide coatings on a substrate.
• the present invention provides a method for forming nano-structured iron oxide coatings on a substrate.
• the method includes the steps of: (a) subjecting a chamber containing a plasma source to vacuum; (b) feeding iron pentacarbonyl and O 2 into a chamber containing a plasma source, wherein the O 2 is fed into the chamber at a rate greater than that of the iron pentacarbonyl; (c) subjecting the substrate to the chamber, wherein the substrate is at a temperature less than 250° C., thereby forming an iron oxide coating on the substrate, wherein the iron oxide is greater than 90 percent in the ⁇ -hematite form.
• the iron oxide coating formed by the method of the present invention is typically greater than 90 percent a-hematite. Oftentimes, at least 95 percent or 97.5 percent of the material is a-hematite.
• the iron oxide materials do not include a significant amount of either magnetite or maghemite forms of iron oxide. They typically contain less than 10 percent magnetite and/or maghemite, and oftentimes they contain less than 5 percent magnetite and/or maghemite.
• the surface of the coatings of the iron oxide materials typically exhibit individual structures (e.g., disc-like structures, box-like structures, diamond-like structures, etc.) that lie in a non-parallel orientation (e.g., vertical) with respect to the substrate plane.
• Such structures typically have a ratio of long dimension to short dimension of at least 2:1. Oftentimes the ratio is at least 3:1 or 4:1. In certain cases, the ratio is at least 5:1 or 6:1.
• the iron oxide coatings typically contain at least 10 individual structures on their surface within a 0.25 ⁇ m 2 area. Oftentimes, the coatings contain at least 25 or 50 disc-like structures on their surface within a 0.25 ⁇ m 2 area.
• Iron pentacarbonyl and O 2 are fed into a chamber, containing a plasma source, through two separate feed lines.
• the O 2 is fed in at a rate at least 4 times greater than that of the iron pentacarbonyl.
• the chamber is subjected to vacuum prior to deposition and maintained under vacuum throughout the procedure.
• a substrate is subjected to the chamber, resulting in the production of an iron oxide coating on the substrate. During the deposition, the substrate is at a temperature less than 250° C.
• the plasma source is typically a high density plasma source, and it is oftentimes an argon plasma source.
• O 2 is fed into the chamber at a rate at least 8 times greater than that of the iron pentacarbonyl, and oftentimes it is fed at a rate at least 12 times greater.
• the chamber is typically subjected to a vacuum of at least 0.10 torr, and, in some cases, to a vacuum of at least 0.01 torr or even 0.005 torr.
• Substrates may be of any suitable composition. Nonlimiting examples include a spectrally transparent cyclic-olefin copolymer, pure poly(norbomene), and a conducting glass plate having an F-doped SnO 2 overlayer.
• the substrate temperature during the deposition is usually less than 200° C. In certain cases it may be less than 175° C., 150° C., or 125° C.
• Substrates are usually passed through the chamber during the coating process at a rate of at least 1 mm/s. Oftentimes, the substrates are passed through at a rate of at least 3 mm/s, 5 mm/s, or even 7 mm/s. Iron oxide coatings on the substrate are typically greater than 90 percent in the ⁇ -hematite form. In certain cases, the coatings are greater than 95 percent or even 97.5 percent in the ⁇ -hematite form. Coating thicknesses on the substrate usually exceed 500 ⁇ , and can exceed 750 ⁇ or even 1000 ⁇ .
• Plasma Source High density.
• Plasma Source High density.
• Plasma Source High density.
• Plasma Source High density.
• Plasma Source High density argon.
• Plasma Source High density argon.
• Plasma Source High density argon.
• Plasma Source High density argon.
• Plasma Source High density argon.
• Plasma Source High density argon.
• a sheet of Topas cyclic olefin copolymer was coated with iron oxide in the following manner.
• Iron pentacarbonyl and O 2 were fed into a chamber, containing a high density argon plasma source operating at 3000 W (Sencera, Charlotte, N.C.), at a rate of 20 sccm and 240 sccm respectively through two separate feed lines.
• the chamber was pumped down to 0.005 Torr prior to deposition and maintained at that pressure throughout the process.
• the sheet which was at a temperature of 140° C., was passed over the feed outlets on a moving carriage at a speed of 5 mm/s to achieve an iron oxide deposit thickness of 1500 ⁇ .
• An XRD pattern of the film showed it was an exact match for a-hematite iron oxide.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Mechanical Engineering (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Materials Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Physics & Mathematics (AREA)
• Plasma & Fusion (AREA)
• Chemical Vapour Deposition (AREA)
• Compounds Of Iron (AREA)
• Laminated Bodies (AREA)

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Cited By (6)

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Citations (97)

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• 2007
  • 2007-03-02 WO PCT/US2007/063213 patent/WO2007103812A1/fr not_active Ceased
  • 2007-03-02 US US11/681,669 patent/US20080038482A1/en not_active Abandoned

Patent Citations (99)

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