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WO2007103812A1 - Method for low temperature production of nano-structured iron oxide coatings - Google Patents

Method for low temperature production of nano-structured iron oxide coatings Download PDF

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Publication number
WO2007103812A1
WO2007103812A1 PCT/US2007/063213 US2007063213W WO2007103812A1 WO 2007103812 A1 WO2007103812 A1 WO 2007103812A1 US 2007063213 W US2007063213 W US 2007063213W WO 2007103812 A1 WO2007103812 A1 WO 2007103812A1
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WIPO (PCT)
Prior art keywords
substrate
iron oxide
plasma source
chamber
iron
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.)
Ceased
Application number
PCT/US2007/063213
Other languages
French (fr)
Inventor
Fred Ratel
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.)
Altairnano Inc
Original Assignee
Altair Nanomaterials Inc
Altairnano Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Altair Nanomaterials Inc, Altairnano Inc filed Critical Altair Nanomaterials Inc
Publication of WO2007103812A1 publication Critical patent/WO2007103812A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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 0 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 ⁇ -hematite. Oftentimes, at least 95 percent or 97.5 percent of the material is ⁇ -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 pecent 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 0 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(norbornene), and a conducting glass plate having an F-doped SnO 2 overlayer.
  • the substrate temperature during the deposition is usually less than 200 0 C. In certain cases it may be less than 175 0 C, 150 0 C, or 125 0 C.
  • Substrates are usually passed through the chamber during the coating process at a rate of at least lmm/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 A, and can exceed 750 A or even 1000 A.
  • Plasma Source High density.
  • O 2 Feed Rate At least 50 seem.
  • Iron Pentacarbonyl Feed Rate At least 10 seem.
  • Chamber Pressure Less than 0.1 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer.
  • Substrate Temperature Less than 250 0 C.
  • Iron Oxide Form Greater than 90 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 500 A.
  • Plasma Source High density.
  • O 2 Feed Rate At least 75 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.1 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer. Substrate Temperature: Less than 250 0 C. Iron Oxide Form: Greater than 90 percent ⁇ -hematite. Iron Oxide Coating Thickness: Greater than 500 A. 3. Plasma Source: High density. O 2 Feed Rate: At least 75 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.1 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer.
  • Substrate Temperature Less than 200 0 C.
  • Iron Oxide Form Greater than 90 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 500 A.
  • Plasma Source High density.
  • O 2 Feed Rate At least 75 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.1 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer.
  • Substrate Temperature Less than 175 0 C.
  • Iron Oxide Form Greater than 90 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 500 A.
  • Plasma Source High density argon.
  • O 2 Feed Rate At least 100 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.01 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer. Substrate Temperature: Less than 175 0 C. Iron Oxide Form: Greater than 95 percent ⁇ -hematite. Iron Oxide Coating Thickness: Greater than 500 A. Substrate Pass-Through Rate: At least 3 mm/s. . Plasma Source: High density argon. O 2 Feed Rate: At least 150 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.01 torr.
  • Substrate Composition Spectrally transparent cyclic-olefm polymer.
  • Substrate Temperature Less than 150 0 C.
  • Iron Oxide Form Greater than 95 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 750 A.
  • Substrate Pass-Through Rate At least 3 mm/s.
  • Plasma Source High density argon.
  • O 2 Feed Rate At least 150 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.01 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer.
  • Substrate Temperature Less than 150 0 C.
  • Iron Oxide Form Greater than 95 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 1000 A.
  • Substrate Pass-Through Rate At least 3 mm/s.
  • Plasma Source High density argon.
  • O 2 Feed Rate At least 150 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.01 torr.
  • Substrate Composition Spectrally transparent cyclic-olefin polymer.
  • Substrate Temperature Less than 150 0 C.
  • Iron Oxide Form Greater than 95 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 1000 A.
  • Substrate Pass-Through Rate At least 5 mm/s.
  • Plasma Source High density argon.
  • O 2 Feed Rate At least 150 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.01 torr.
  • Substrate Composition Poly(norbornene).
  • Substrate Temperature Less than 150 0 C.
  • Iron Oxide Form Greater than 95 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 1000 A.
  • Substrate Pass-Through Rate At least 5 mm/s.
  • Plasma Source High density argon.
  • O 2 Feed Rate At least 150 seem.
  • Iron Pentacarbonyl Feed Rate At least 15 seem.
  • Chamber Pressure Less than 0.01 torr.
  • Substrate Composition Conducting glass plate having an F-doped SnO 2 overlayer
  • Substrate Temperature Less than 150 0 C.
  • Iron Oxide Form Greater than 95 percent ⁇ -hematite.
  • Iron Oxide Coating Thickness Greater than 1000 A.
  • Substrate Pass-Through Rate At least 5 mm/s.
  • 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, NC), at a rate of 20 seem and 240 seem 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 0 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 A.
  • An XRD pattern of the film showed it was an exact match for ⁇ -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)
  • Laminated Bodies (AREA)
  • Compounds Of Iron (AREA)

Abstract

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 O2 into a chamber containing a plasma source, wherein the O2 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 α-hematite form.

Description

METHOD FOR LOW TEMPERATURE PRODUCTION OF NANO-STRUCTURED
IRON OXIDE COATINGS
Field of the Invention
The present invention provides a method for forming nano-structured iron oxide coatings on a substrate. Background of the Invention
Several techniques are known for depositing iron oxide coatings onto a substrate. Most of the methods, however, are limited in that substrate temperatures greater than 400 0C are used. This is because the oxides are pyrolytically formed on the substrate surface. Such procedures inherently limit the types of substrates that may be used, since substrates melting at the high temperatures are prohibited.
It is accordingly an object of the present invention to provide a method of depositing iron oxide on a substrate at temperatures substantially below 400 0C. Summary of the Invention
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 O2 into a chamber containing a plasma source, wherein the O2 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 0C, thereby forming an iron oxide coating on the substrate, wherein the iron oxide is greater than 90 percent in the α-hematite form. Iron Oxide Coating
The iron oxide coating formed by the method of the present invention, which is undoped, is typically greater than 90 percent α-hematite. Oftentimes, at least 95 percent or 97.5 percent of the material is α-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 pecent 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 μm2 area. Oftentimes, the coatings contain at least 25 or 50 disc-like structures on their surface within a 0.25 μm2 area. Method of Deposition
Iron pentacarbonyl and O2 are fed into a chamber, containing a plasma source, through two separate feed lines. The O2 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 0C.
The plasma source is typically a high density plasma source, and it is oftentimes an argon plasma source. Li certain cases, O2 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(norbornene), and a conducting glass plate having an F-doped SnO2 overlayer. The substrate temperature during the deposition is usually less than 200 0C. In certain cases it may be less than 175 0C, 150 0C, or 125 0C.
Substrates are usually passed through the chamber during the coating process at a rate of at least lmm/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 α-hematite form. In certain cases, the coatings are greater than 95 percent or even 97.5 percent in the α-hematite form. Coating thicknesses on the substrate usually exceed 500 A, and can exceed 750 A or even 1000 A.
The following are non-limiting examples of the method of the present invention:
1. Plasma Source: High density. O2 Feed Rate: At least 50 seem.
Iron Pentacarbonyl Feed Rate: At least 10 seem.
Chamber Pressure: Less than 0.1 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer.
Substrate Temperature: Less than 250 0C.
Iron Oxide Form: Greater than 90 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 500 A.
2. Plasma Source: High density. O2 Feed Rate: At least 75 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem. Chamber Pressure: Less than 0.1 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer. Substrate Temperature: Less than 250 0C. Iron Oxide Form: Greater than 90 percent α-hematite. Iron Oxide Coating Thickness: Greater than 500 A. 3. Plasma Source: High density. O2 Feed Rate: At least 75 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem.
Chamber Pressure: Less than 0.1 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer.
Substrate Temperature: Less than 200 0C.
Iron Oxide Form: Greater than 90 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 500 A.
4. Plasma Source: High density. O2 Feed Rate: At least 75 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem.
Chamber Pressure: Less than 0.1 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer.
Substrate Temperature: Less than 175 0C.
Iron Oxide Form: Greater than 90 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 500 A.
5. Plasma Source: High density argon. O2 Feed Rate: At least 100 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem. Chamber Pressure: Less than 0.01 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer. Substrate Temperature: Less than 175 0C. Iron Oxide Form: Greater than 95 percent α-hematite. Iron Oxide Coating Thickness: Greater than 500 A. Substrate Pass-Through Rate: At least 3 mm/s. . Plasma Source: High density argon. O2 Feed Rate: At least 150 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem.
Chamber Pressure: Less than 0.01 torr.
Substrate Composition: Spectrally transparent cyclic-olefm polymer.
Substrate Temperature: Less than 150 0C.
Iron Oxide Form: Greater than 95 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 750 A.
Substrate Pass-Through Rate: At least 3 mm/s.
7. Plasma Source: High density argon. O2 Feed Rate: At least 150 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem.
Chamber Pressure: Less than 0.01 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer.
Substrate Temperature: Less than 150 0C.
Iron Oxide Form: Greater than 95 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 1000 A.
Substrate Pass-Through Rate: At least 3 mm/s.
8. Plasma Source: High density argon. O2 Feed Rate: At least 150 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem. Chamber Pressure: Less than 0.01 torr.
Substrate Composition: Spectrally transparent cyclic-olefin polymer. Substrate Temperature: Less than 150 0C. Iron Oxide Form: Greater than 95 percent α-hematite. Iron Oxide Coating Thickness: Greater than 1000 A. Substrate Pass-Through Rate: At least 5 mm/s.
9. Plasma Source: High density argon. O2 Feed Rate: At least 150 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem.
Chamber Pressure: Less than 0.01 torr.
Substrate Composition: Poly(norbornene).
Substrate Temperature: Less than 150 0C.
Iron Oxide Form: Greater than 95 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 1000 A.
Substrate Pass-Through Rate: At least 5 mm/s.
10. Plasma Source: High density argon. O2 Feed Rate: At least 150 seem.
Iron Pentacarbonyl Feed Rate: At least 15 seem.
Chamber Pressure: Less than 0.01 torr.
Substrate Composition: Conducting glass plate having an F-doped SnO2 overlayer
Substrate Temperature: Less than 150 0C.
Iron Oxide Form: Greater than 95 percent α-hematite.
Iron Oxide Coating Thickness: Greater than 1000 A.
Substrate Pass-Through Rate: At least 5 mm/s. Example
Example 1
Deposition of Iron Oxide on Cyclic Olefin Copolymer A sheet of Topas cyclic olefin copolymer was coated with iron oxide in the following manner. Iron pentacarbonyl and O2 were fed into a chamber, containing a high density argon plasma source operating at 3000 W (Sencera, Charlotte, NC), at a rate of 20 seem and 240 seem 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 0C, 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 A. An XRD pattern of the film showed it was an exact match for α-hematite iron oxide.

Claims

CLAIMS:
1. A method of forming an iron oxide coating on a substrate, wherein the method comprises the following steps:
(a) subjecting a chamber containing a plasma source to vacuum;
(b) feeding iron pentacarbonyl and O2 into a chamber containing a plasma source, wherein the O2 is fed into the chamber at a rate at least 4 times greater than that of the iron pentacarbonyl;
(c) subjecting the substrate to the chamber, wherein the substrate is at a temperature less than 250 0C thereby forming an iron oxide coating on the substrate, wherein the coating is greater than 500 A thick, and wherein the iron oxide is greater than 90 percent in the α- hematite form.
2. The method according to claim 1 , wherein the iron pentacarbonyl is fed into the chamber at a rate of at least 10 seem.
3. The method according to claim 1, wherein the plasma source is a high density argon plasma source.
4. The method according to claim 1, wherein the substrate comprises a spectrally transparent cyclic olefin polymer.
5. The method according to claim 1, wherein the substrate is at a temperature less than 200 0C.
6. The method according to claim 1, wherein the coating on the substrate is greater than 750 A thick.
7. The method according to claim 1, wherein the iron oxide coating is greater than 95 percent in the α-hematite form.
8. The method according to claim 1, wherein the O2 is fed into the chamber at a rate at least 8 times greater than that of the iron pentacarbonyl.
9. The method according to claim 8, wherein the plasma source is a high density argon plasma source.
10. The method according to claim 9, wherein the substrate is at a temperature less than 175 0C.
PCT/US2007/063213 2006-03-02 2007-03-02 Method for low temperature production of nano-structured iron oxide coatings Ceased WO2007103812A1 (en)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
US77872906P 2006-03-02 2006-03-02
US77873006P 2006-03-02 2006-03-02
US60/778,730 2006-03-02
US60/778,729 2006-03-02
US81140306P 2006-06-05 2006-06-05
US60/811,403 2006-06-05

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US20080020175A1 (en) * 2006-03-02 2008-01-24 Fred Ratel Nanostructured Indium-Doped Iron Oxide
US20080044638A1 (en) * 2006-03-02 2008-02-21 Fred Ratel Nanostructured Metal Oxides
US20080254258A1 (en) * 2007-04-12 2008-10-16 Altairnano, Inc. Teflon® replacements and related production methods
ITPD20110285A1 (en) 2011-09-08 2013-03-09 Univ Padova METHOD FOR PREPARING NANOMATERIALS SUPPORTED BY IRON OXID (III) BASED ON CVD TECHNIQUE AND FE SYNTHESIS METHOD (HFA) 2TMEDA

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