WO2007103812A1 - Procédé de production à basse température de revêtements d'oxyde de fer nanostructurés - Google Patents
Procédé de production à basse température de revêtements d'oxyde de fer nanostructurés Download PDFInfo
- 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
- Authority
- WO
- 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
Links
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
La présente invention concerne un procédé de formation de revêtements d'oxyde de fer nanostructurés sur un substrat. Le procédé comprend les étapes consistant: (a) à soumettre une chambre contenant une source de plasma à un vide; (b) à alimenter du fer pentacarbonyle et de l'O2 dans une chambre contenant une source de plasma, l'O2 étant alimenté dans la chambre à un débit supérieur à celui du fer pentacarbonyle; (c) à placer le substrat dans la chambre, le substrat étant à une température inférieure à 250°C, permettant ainsi de former un revêtement d'oxyde de fer sur le substrat, l'oxyde de fer se présentant à plus de 90% sous la forme d'hématite alpha.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US77873006P | 2006-03-02 | 2006-03-02 | |
| US77872906P | 2006-03-02 | 2006-03-02 | |
| US60/778,729 | 2006-03-02 | ||
| US60/778,730 | 2006-03-02 | ||
| US81140306P | 2006-06-05 | 2006-06-05 | |
| US60/811,403 | 2006-06-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2007103812A1 true WO2007103812A1 (fr) | 2007-09-13 |
Family
ID=38475201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US2007/063213 Ceased WO2007103812A1 (fr) | 2006-03-02 | 2007-03-02 | Procédé de production à basse température de revêtements d'oxyde de fer nanostructurés |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US20080038482A1 (fr) |
| WO (1) | WO2007103812A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014055750A1 (fr) | 2012-10-05 | 2014-04-10 | Basf Corporation | Pigments à effet contenant de l'oxyde de fer, fabrication et utilisation associées |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101001610A (zh) * | 2004-07-13 | 2007-07-18 | 爱尔达纳米公司 | 防止药物转向的陶瓷结构 |
| CA2620167A1 (fr) * | 2005-08-23 | 2007-03-01 | Altairnano, Inc. | Composition d'anatase-tio2 dopee au phosphore hautement catalytique et methodes de fabrication connexes |
| US20080044638A1 (en) * | 2006-03-02 | 2008-02-21 | Fred Ratel | Nanostructured Metal Oxides |
| WO2007103820A1 (fr) * | 2006-03-02 | 2007-09-13 | Altairnano, Inc. | Oxyde de fer dopé à l'indium nanostructuré |
| US20080254258A1 (en) * | 2007-04-12 | 2008-10-16 | Altairnano, Inc. | Teflon® replacements and related production methods |
| ITPD20110285A1 (it) | 2011-09-08 | 2013-03-09 | Univ Padova | Metodo per preparare nanomateriali supportati a base di ossido di ferro (iii) con tecnica cvd e metodo di sintesi di fe(hfa)2tmeda |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014055750A1 (fr) | 2012-10-05 | 2014-04-10 | Basf Corporation | Pigments à effet contenant de l'oxyde de fer, fabrication et utilisation associées |
| EP2904053A4 (fr) * | 2012-10-05 | 2016-05-04 | Basf Corp | Pigments à effet contenant de l'oxyde de fer, fabrication et utilisation associées |
| US9951194B2 (en) | 2012-10-05 | 2018-04-24 | Basf Corporation | Iron oxide containing effect pigments, their manufacture and their use |
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|---|---|
| US20080038482A1 (en) | 2008-02-14 |
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