WO2008057710A2 - Method for coating a substrate and coated product - Google Patents
Method for coating a substrate and coated product Download PDFInfo
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- WO2008057710A2 WO2008057710A2 PCT/US2007/081200 US2007081200W WO2008057710A2 WO 2008057710 A2 WO2008057710 A2 WO 2008057710A2 US 2007081200 W US2007081200 W US 2007081200W WO 2008057710 A2 WO2008057710 A2 WO 2008057710A2
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Classifications
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- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31678—Of metal
Definitions
- the present invention relates to a method of applying coatings which contain only small amounts of different gaseous impurities, in particular oxygen and hydrogen.
- tungsten and copper impurities which originate from the electrodes used, are introduced into the coating, which is generally undesirable, in the case of, for example, the use of tantalum or niobium coatings for corrosion protection, such impurities reduce the protective effect of the coating by the formation of so-called micro-galvanic cells.
- WO-A-03/106,051 discloses a method and an apparatus for low pressure cold spraying. In this process a coating of powder particles is sprayed in a gas substantially at ambient temperatures onto a workpiece. The process is conducted in a low ambient pressure environment which is less than atmospheric pressure to accelerate the sprayed_powder particles. With this process a coating of a powder is formed on a workpiece.
- EP-A- 1 ,382,720 discloses another method and apparatus for low pressure cold spraying.
- the target to be coated and the cold spray gun are located within a vacuum chamber at pressures below 80 kPa. With this process a workpiece is coated with a powder.
- Another object of this invention was the provision of a novel process for 5 preparing dense and corrosion resistant coatings, especially tantalum coatings, which possess low content of impurities, preferably low content of oxygen, hydrogen and nitrogen impurities, which coatings are highly qualified for use as corrosion protective layer, especialiy in equipment of chemical plants.
- the object of the present invention is achieved by applying a desired refractory metal to the desired surface by a method as claimed in claim 1.
- cold spray process or the kinetic spray process are particularly suitable for the method according to the invention; the cold spray process, which is described in EP-A-484533, is especially suitable, and this specification is incorporated herein by reference.
- a powder of a materia! selected from the group consisting of niobium, tantalum, tungsten, mo
- the metal powder particles striking the surface of the object form a coating, the particles being deformed very considerably.
- the powder particles are advantageously present in the jet in an amount that ensures a flow rate density of the particles of from 0.01 to 200 g/s cm 2 , preferably 0.01 to 100 g/s cm 2 , very preferably 0.01 g/s cm 2 to 20 g/s cm 2 , or most preferred from 0.05 g/s cm 2 to 17 g/s cm 2 .
- a powder feed rate of, for example, 70 g/min 1.1667 g/s is a typical example of a powder feed rate.
- an inert gas such as argon, neon, helium, nitrogen or mixtures of two or more thereof.
- air may also be used, if safety regulations are met also use of hydrogen or mixtures of hydrogen with other gases can be used,
- the spraying comprises the steps of:
- a powder of a particulate material chosen from the group consisting of niobium, tantalum, tungsten, molybdenum, titanium, zirconium, nickel, cobalt, iron, chromium, o aluminium, silver, copper, mixtures of at least two thereof or alloys thereof with one another or other metals, the powder having a particle size of 0.5 to 150 ⁇ m, an oxygen content of iess than 500 ppm oxygen and a hydrogen content of less than 500 ppm, said powder being under pressure; 5 - providing an inert gas under pressure to the spraying orifice to establish a static pressure at the spraying orifice and providing a spray of said particulate material and gas onto the surface to be coated; and
- the spraying is performed with a cold spray gun and the target to be coated and the cold spray gun are located 5 within a vacuum chamber at pressures below 80 kPa, preferably between 0.1 and 50 kPa, and most preferred between 2 and 10 kPa.
- the metat has a purity of 99% or more, such as 99.5% or 99.7% or
- the metai advantageously has a purity of at least 99.95%, based on metallic impurities, especially of at least 99.995% or of at least 99.999%, in particular of at least 99.9995%.
- the metal powder has a content of less than 500 ppm oxygen, or less than 300 ppm, in particular an oxygen content of less than 100 ppm, and a content of less than 500 ppm hydrogen, or a hydrogen content of less than 300 ppm, in particular a hydrogen content of less than 100 ppm. 5
- the amount of these impurities in the starting powders is very low, then the deposition efficiency of the powders increases and the density of the applied coatings is increased.
- Particularly suitable refractory metal powders have a purity of at least 99.7%, o advantageously of at least 99.9%, in particular 99.95%, a content of less than 500 ppm oxygen, or less than 300 ppm oxygen, in particular an oxygen content of less than 100 ppm and a content of less than 500 ppm hydrogen, or less than 300 ppm hydrogen, in particular a hydrogen content of less than 100 ppm.
- Particularly suitable refractory metal powders have a purity of at least 99.95%, in particular of at least 99.995%, and a content of less than 500 ppm oxygen, or less than 300 ppm oxygen, in particular an oxygen content of less than 100 ppm and a content of less than 500 ppm hydrogen, or less than 300 ppm hydrogen, in particular a hydrogen content of less than 100 ppm.
- Particularly suitable metal powders have a purity of at least 99.999%, in particular of at least 99.9995%, and a content of less than 500 ppm oxygen, or less than 300 ppm oxygen, in particular an oxygen content of less than 100 ppm and a content of less than 500 ppm hydrogen, or less than 300 ppm hydrogen, in particular a hydrogen content of less than 100 ppm.
- the total content of other non-metallic impurities should advantageously be less than 500 ppm, preferably less than 150 ppm.
- the oxygen content is advantageously 50 ppm or less
- the hydrogen content is 50 ppm or less
- the nitrogen content is 25 ppm or less
- the carbon content is 25 ppm or less.
- the content of metallic impurities is advantageously 500 ppm or less, preferably 100 ppm or less and most preferably 50 ppm or less, in particular 10 ppm or less.
- Preferred suitable metal powders are, for example, many of the refractory metal powders which are also suitable for the production of capacitors.
- Such metal powders can be prepared by reduction of refractory metal compound with a reducing agent and preferably subsequent deoxidation.
- Tungsten oxide or molybdenum oxide for example, is reduced in a stream of hydrogen at elevated temperature.
- the preparation is described, for example, in Schubert, Lassner, 'Tungsten", Kluwer Academic/Plenum Publishers, New York, 1999 or Brauer, "Handbuch der Praparativen Anorganischen Chemie", originally Enke Verlag Stuttgart, 1981 , p 1530.
- the preparation in most cases carried out by reducing alkali heptafluorotantalates and earth alkaline metal heptafluoro-tantalates or the oxides, such as, for example, sodium heptafluorotantalate, potassium heptafiuorotantalate, sodium heptafluorontobate or potassium heptafluoroniobate, with an alkali or alkaline earth metal.
- the reduction can be carried out in a salt melt with the addition of, for example, sodium, or in the gas phase, calcium or magnesium vapour advantageously being used.
- deoxidation is preferably carried out. This can be effected, for example, by mixing the refractory metal powder with Mg, Ca, Ba, La, Y or Ce and then heating, or by heating the refractory metal in the presence of a getter in an atmosphere that allows oxygen to pass from the metal powder to the getter.
- the refractory metal powder is in most cases then freed of the salts of the deoxidising agent using an acid and water, and is dried.
- the metallic impurities can be kept low.
- a further process for preparing pure powder having a low oxygen content consists in reducing a refractory metal hydride using an alkaline earth metal as reducing agent, as disclosed, for example, in WO 01/12364 and EP-A-
- the thickness of the coating is usually more than 0.01 mm. Preferred are layers with a thickness between 0.05 and 10 mm, more preferred between 0.05 and 5 mm, still more preferred between 0,05 and 1 mm, still more preferred between
- the purities and oxygen and hydrogen contents of the resulting coatings should deviate not more than 50 % and preferably not more than 20% from those of the powder.
- this can be achieved by coating the substrate surface under an inert gas.
- Argon is advantageously used as the inert gas because, owing to its higher density than air, it tends to cover the object to be coated and to remain present, in particular when the surface to be coated is located in a vessel which prevents the argon from escaping or flowing away and more argon is continuously added.
- the coatings applied according to the invention have a high purity and a low oxygen content and a low hydrogen content.
- these coatings have an oxygen content of less than 500, or less than 300, in particular an oxygen content of less than 100 ppm and a hydrogen content of less than 500, or less than 300, in particular an hydrogen content of less than 100 ppm.
- these coatings have a purity of at least 99.7%, advantageously of at least 99.9%, in particular of at least 99.95%, and a content of less than 500 ppm oxygen, or less than 300 ppm oxygen, in particular an oxygen content of less than 100 ppm, and have a hydrogen content of less than 500, or less than 300, in particular a hydrogen content of less than 100 ppm.
- these coatings have a purity of at least 99.95%, in particular of at least 99.995%, and a content of less than 500 ppm oxygen, or less than 300 ppm oxygen, in particular an oxygen content of less than 100 ppm and have a hydrogen content of less than 500, or less than 300, in particular a hydrogen content of less than 100 ppm.
- these coatings have a purity of 99.999%, in particular of at least 99.9995%, and a content of less than 500 ppm oxygen, or less than 300 ppm oxygen, in particular an oxygen content of iess than 100 ppm and have a hydrogen content of less than 500, or less than 300, in particular a hydrogen 5 content of less than 100 ppm.
- the coatings according to the invention have a total content of other non- metat ⁇ c impurities, such as carbon, nitrogen or hydrogen, which is advantageously below 500 ppm and most preferably below 150 ppm. 0
- the applied coating has a content of gaseous impurities which differs by not more than 50%, or not more than 20%, or not more than 10%, or not more than 5%, or not more than 1 %, from the content of the starting powder with which this coating was produced.
- the term "differs" is to be understood as meaning in5 particular an increase; the resulting coatings should, therefore, advantageously have a content of gaseous impurities that is not more than 50% greater than the content of the starting powder.
- the applied coating preferably has an oxygen content which differs by not more o than 5%, in particular not more than 1 %, from the oxygen content of the starting powder and has a hydrogen content which differs by not more than 5%, in particular not more than 1 %, from the hydrogen content of the starting powder.
- the coatings according to the invention preferably have a total content of other5 non-metaliic impurities, such as carbon or nitrogen, which is advantageously less than 500 ppm and most preferably less than 150 ppm. With the process of this invention layers with higher impurity contents can also be produced.
- the oxygen content is advantageously 50 ppm or less
- the o hydrogen content is advantageously 50 ppm or less
- the nitrogen content is 25
- the content of metallic impurities is advantageously 50 ppm or less, in particular 10 ppm or less.
- the coatings additionally have a density of at least 97%, preferably greater than 98%, in particular greater than 99% or 99.5%.
- 97 % density of a layer means that the layer has a density of 97 % of the bulk material.
- the density of the coating is here a measure of the closed nature and porosity of the coating.
- a closed, substantially pore-free coatingo always has a density of more than 99.5%.
- the density can be determined either by image analysis of a cross-sectional image (ground section) of such a coating, or alternatively by helium pycnometry.
- the density can be determined by first determining the total area of the coating to be investigated in the image area of the microscope and relating this area to the areas of the pores. In this method, pores that are located far from the surface and close to the interface with the substrate are aiso detected.
- the coatings show high mechanical strength which is caused by their high density and by the high deformation of the particles.
- the strengths are at least 80 MPa more preferably at least 100 MPa, most preferably at least 140 MPa when nitrogen is used as the gas with which the metal powder forms a gas-powder mixture.
- the strength usually is at least 150 MPa, preferably at least 170 MPa, most preferably at least 200 MPa and very most preferred greater than 250 MPa.
- the articles to be coated with the process of this invention are not limited. Generally all articles which need a coating, preferably a corrosion protective coating, can be used. These articles may be made of metal and/or of ceramic material and/or of plastic materia! or may comprise components from these materials. Preferably surfaces of materials are coated which are subject to removal of material, for example by wear, corrosion, oxidation, etching, machining or other stress.
- Preferably surfaces of materials are coated with the process of this invention which are used in corroding surroundings, for example in chemical processes in medical devices or in implants.
- apparatus or components to be coated are components used in chemical plants or in laboratories or in medical devices or as implants, such as reaction and mixing vessels, stirrers, bund flanges, thermowells, birsting disks, birsting disk holders, heat exchangers (shell and tubes), pipings, vaives, valve bodies, sputter targets, X-ray anode plates, preferably X-ray rotating anodes, and pump parts.
- the coatings prepared with the process of this invention preferably are used in corrosion protection.
- the present invention therefore relates also to articles made of metal and/or of ceramic material and/or of plastic material containing at least one coatings composed of the metals niobium, tantalum, tungsten, molybdenum, titanium, zirconium, nickel, cobalt, iron, chromium, aluminium, silver, copper, or mixtures of two or more thereof or alloys of two or more thereof or alloys with other metals, which coatings have the above-mentioned properties.
- Such coatings are in particular coatings of tantalum or niobium.
- layers of tungsten, molybdenum, titanium zirconium or mixtures of two or more thereof or alloys of two or more thereof or alloys with other metals are applied by cold spraying to the surface of a substrate to be coated.
- said powders or powder mixtures preferably with tantalum and niobium powders, possessing a reduced oxygen content below 500 ppm and a reduced hydrogen content below 500 ppm, there can be produced cold sprayed layers with very high deposition rates of more than 90 %.
- Suitable metal powders for use in the methods according to the invention are also metal powders that consist of alloys, pseudo alioys and powder mixtures of refractory metals with suitable non-refractory metals.
- alloys include especially alloys, pseudo alloys or powder mixtures of a metal selected from the group consisting of niobium, tantalum, tungsten, molybdenum, titanium, zirconium, nickel, cobalt, iron, chromium, aluminium, silver, copper, or mixtures of two or more thereof, with a metal selected from the group rhodium, palladium, platinum and gold.
- Such powders belong to the prior art, are known in principle to the person skilled in the art and are described, for example, in EP-A-774315 and EP-A-1138420.
- AHoy powders are in most cases obtainable by melting and mixing the alloying partners. According to the invention there may be used as alloy powders also so-called pre-alloyed powders. These are powders which are produced by mixing compounds such as, for example, salts, oxides and/or hydrides of the alloying partners and then reducing them, so that intimate mixtures of the metals in question are obtained. It is additionally possible according to the invention to use pseudo alloys. Pseudo alloys are understood as being materials which are obtained not by conventional melt metallurgy but, for example, by grinding, sintering or infiltration.
- tungsten/copper alloys or tungsten/copper mixtures, the properties of which are known and are listed here by way of example:
- molybdenum-copper alloys or molybdenium / copper mixtures in the same ratios as indicated above.
- molybdenum-silver alloys or molybdenium/ silver mixtures which contain, for example, 10, 40 or 65 wt.% molybdenum.
- tungsten-silver alloys or tungsten /silver mixtures which 5 contain, for example, 10, 40 or 65 wt.% tungsten.
- nickel-chromium alloys or nickel-chromium mixtures which contain, for example, 80 wt.% nickel. o These can be used, for example, in heat pipes, cooling bodies or, in general, in temperature management systems.
- tungsten-rhenium alloys or mixtures or the metal powder is an alloy having the following composition: 5 from 94 to 99 wt.%, preferably from 95 to 97 wt.%, molybdenum, from 1 to 6 wt.%, preferably from 2 to 4 wt.%, niobium, from 0.05 to 1 wt.%, preferably from 0.05 to 0.02 wt.%, zirconium.
- alloys like pure metal powders having a purity of at least 99.95 %, can be used in the recycling or production of sputter targets by means of cold gas spraying.
- Figure 1 illustrates the velocity of Ta particles sprayed using different gases and parameters.
- Figure 2 illustrates TCT strength and cavitation rate of Ta coatings.
- Figure 3 illustrates deposition efficiency of Ta and Nb powders.
- Figure 4 illustrates the deposition efficiency of Nt at different temperatures using N 2 and a pressure of 3,3 MPa
- Figure 5 illustrates light microscope pictures of unetched Ta coatings.
- coatings made from Ta 1 AMPERIT ® 150 standard using helium is shown
- Figure 5b coatings made from Ta, AMPERIT ® 151 , optimised using nitrogen is shown
- Figure 5c coatings made from Ta, AMPERIT ® 151 , optimised using helium is shown.
- Figure 6 illustrates tight microscope pictures of the Ta coatings of Figure 5 that have been etched.
- the coatings of Figures 6a, 6b and 6c correspond to the coatings of Figures 5a, 5b and 5c.
- Figure 7 illustrates Ta coatings sprayed on mild steel after corrosion testing.
- a coating after salt spray test Ta, standard, He , after 168 h is shown;
- a coating after salt spray test Ta, optimised, N 2 after 1008 h is shown;
- Figure 7c the surface of a coating after an emerging test (28 days, 20% HCI 1 7O 0 C): Ta, optimised, N 2 is shown;
- Figure 7d the cross section of the coating of Figure 7c is shown within the test area.
- Tantalum and niobium coatings were produced.
- the metal powders used are i o indicated in the table above. These powders are commerciaiiy available from H. C. Starck GmbH & Co.KG in Goslar,
- Ni As an example it is shown that very simiiar modifications can be successfully performed for non refractory metais, too.
- Ni powders for thermal spraying are produced by water atomising resulting in a partially irregular morphology of such a powder.
- water atomised Ni powders contain a high oxygen content of about 0,18 wt.%.
- the optimised powder has been produced by gas atomisation and contains only 180 ppm oxygen, which is only 10% compared to the water atomised powder.
- the powder particles are predominantly spherical.
- the spray tests illustrate that for both powders the deposition efficiency raises when the gas temperature is increased. However, the deposition efficiency is about 20 % higher when the optimised Ni powder AMPERIT ® 176 is used and reaches values of over 90 % at 600 0 C.
- the coatings sprayed from this optimised powder exhibit a higher density and the particles show higher deformation as well as better bonding to each other.
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Powder Metallurgy (AREA)
- Coating By Spraying Or Casting (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
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Priority Applications (14)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2009536369A JP5377319B2 (en) | 2006-11-07 | 2007-10-12 | Substrate coating method and coated product |
BRPI0718237-6A2A BRPI0718237A2 (en) | 2006-11-07 | 2007-10-12 | METHOD FOR COATING A SUBSTRATE SURFACE AND COATED PRODUCT |
RU2009121447/02A RU2469126C2 (en) | 2006-11-07 | 2007-10-12 | Method of applying coating on substrate surface and coated product |
NZ576664A NZ576664A (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate surface and coated product |
CA2669052A CA2669052C (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product |
US12/513,715 US20100015467A1 (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product |
CN200780040963.2A CN101730757B (en) | 2006-11-07 | 2007-10-12 | The method of coated substrate surface and the product through coating |
EP07868426.3A EP2104753B1 (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product |
AU2007317650A AU2007317650B2 (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product |
PL07868426T PL2104753T3 (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product |
MX2009004773A MX2009004773A (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product. |
DK07868426T DK2104753T3 (en) | 2006-11-07 | 2007-10-12 | PROCEDURE FOR COATING A SUBSTRATE AND A COATED PRODUCT |
IL19826809A IL198268A (en) | 2006-11-07 | 2009-04-21 | Method for coating a substrate and coated product |
NO20091959A NO20091959L (en) | 2006-11-07 | 2009-05-20 | Process for coating a substrate and a coated product |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US86472906P | 2006-11-07 | 2006-11-07 | |
US60/864,729 | 2006-11-07 |
Publications (3)
Publication Number | Publication Date |
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WO2008057710A2 true WO2008057710A2 (en) | 2008-05-15 |
WO2008057710A9 WO2008057710A9 (en) | 2009-08-06 |
WO2008057710A3 WO2008057710A3 (en) | 2009-10-15 |
Family
ID=39295597
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2007/081200 WO2008057710A2 (en) | 2006-11-07 | 2007-10-12 | Method for coating a substrate and coated product |
Country Status (16)
Country | Link |
---|---|
US (1) | US20100015467A1 (en) |
EP (1) | EP2104753B1 (en) |
JP (1) | JP5377319B2 (en) |
CN (1) | CN101730757B (en) |
AU (1) | AU2007317650B2 (en) |
BR (1) | BRPI0718237A2 (en) |
CA (1) | CA2669052C (en) |
DK (1) | DK2104753T3 (en) |
IL (1) | IL198268A (en) |
MX (1) | MX2009004773A (en) |
NO (1) | NO20091959L (en) |
NZ (1) | NZ576664A (en) |
PL (1) | PL2104753T3 (en) |
RU (1) | RU2469126C2 (en) |
WO (1) | WO2008057710A2 (en) |
ZA (1) | ZA200902935B (en) |
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Also Published As
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ZA200902935B (en) | 2010-07-28 |
CN101730757B (en) | 2015-09-30 |
PL2104753T3 (en) | 2014-12-31 |
CA2669052C (en) | 2013-11-26 |
WO2008057710A3 (en) | 2009-10-15 |
CA2669052A1 (en) | 2008-05-15 |
AU2007317650A1 (en) | 2008-05-15 |
RU2469126C2 (en) | 2012-12-10 |
EP2104753A2 (en) | 2009-09-30 |
BRPI0718237A2 (en) | 2013-11-12 |
NO20091959L (en) | 2009-06-03 |
WO2008057710A9 (en) | 2009-08-06 |
AU2007317650B2 (en) | 2012-06-14 |
MX2009004773A (en) | 2009-05-21 |
IL198268A (en) | 2015-02-26 |
JP2010509502A (en) | 2010-03-25 |
RU2009121447A (en) | 2010-12-20 |
JP5377319B2 (en) | 2013-12-25 |
DK2104753T3 (en) | 2014-09-29 |
CN101730757A (en) | 2010-06-09 |
NZ576664A (en) | 2012-03-30 |
EP2104753B1 (en) | 2014-07-02 |
IL198268A0 (en) | 2009-12-24 |
US20100015467A1 (en) | 2010-01-21 |
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