• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    There is disclosed a method of forming an oxide coating for reducing the accumulation of radioactive species on a metal surface exposed to fluids containing charged particles. The method comprises preparing an aqueous colloidal suspension containing from about 0.5% to about 35% by weight nanoparticles containing titanium oxide and / or zirconia and from about 0.1% to about 10% 2- [2- (2-methoxyethoxy ) ethoxy] -acetic acid (C 7 H 14 O 5) or polyfluorosulfonic acid in water, depositing the aqueous colloidal suspension on the metal surface, drying the aqueous colloidal suspension to form an unsintered coating; and then heating the unsintered coating to a temperature of up to 500 ° C to densify the unsintered coating and to form an oxide coating having a zeta potential that is less than or equal to the electrical polarity of the charged particles, so to minimize the deposition of the charged particles on the metal surface. The nanoparticles have a diameter of up to about 200 nanometers.
    公开号:CH705093B1
    申请号:CH00792/12
    申请日:2012-06-06
    公开日:2016-05-13
    发明作者:Jin Kim Young；Yu-Chung Ku Anthony；Christine Malish Rebecca；Alfred Caine Thomas；Denault Lauraine；Thomas Barbuto Anthony；Procik Dulka Catherine；Daniel Willson Patrick；Louis Andresen Peter
    申请人:Gen Electric；
    IPC主号:
    专利说明:

    State of the art
    The invention generally relates to coatings and methods for their order. More particularly, the invention relates to a ceramic coating for use in an aqueous environment to prevent accumulation of deposition material on metal surfaces within the aqueous environment, and a method of forming the ceramic coating using a colloid based process such that the ceramic coating is dense is, has a controlled thickness and has a zeta potential that is less than or equal to the electrical polarity of the respective major deposits.
    Components exposed to a high temperature aqueous environment, for example nozzles and throat areas of jet pump assemblies, impellers, condenser tubes, recirculation pumps and steam generator parts in boiling water nuclear reactors, are subject to fouling resulting from charged particles in the hot coolant (usually water from about 100 to about 300 ° C) deposited on metal surfaces of the components. Over time, fouling results in the formation of a thick, dense oxide "crud" layer on the exposed surfaces of the component. The accumulation of fouling agents is a difficult operating and maintenance problem for, for example, boiling water nuclear reactors, because the accumulation of fouling agents substantially improves the efficiency of the coolant recirculation system of a reactor by reducing flow rates of the coolant (water) and reducing the performance of the cooling system decreases. In addition to the accumulation of fouling agents, components are also susceptible to the accumulation of radioactive material on their surfaces, for example radioactive particles of cobalt, carried in the coolant. Fouling agents are normally removed from the surfaces of the components of the boiling water nuclear reactor during the scheduled shutdown of the reactor. However, this approach is costly and does not help maintain the efficiency of the coolant recirculation system between shutdowns. It would therefore be desirable to develop a coating that is particularly well-suited to minimize or eliminate fouling rates on the surfaces exposed to a high temperature water environment.
    Brief description of the invention
    [0003] The inventors of the present patent application have solved the problem of minimizing or eliminating the fouling rate on components exposed to high temperature water environments by developing a water-based coating and a method of applying the coating to component surfaces to control the fouling rate of radioactive particle types minimize or eliminate the component surface.
    Briefly, a process according to one embodiment forms an oxide coating on a metal surface to reduce the deposition of charged particles on the metal surface when in contact with a coolant containing the charged particles. The process comprises preparing an aqueous colloidal suspension containing from about 0.5% to about 35% by weight nanoparticles containing titanium oxide and / or zirconium oxide, depositing the aqueous colloidal suspension onto the metal surface, drying the aqueous colloidal suspension to an unsintered one Coating and then heating the unsintered coating to a temperature of up to 500 ° C to densify the unsintered coating and to obtain the oxide coating having a zeta potential that is less than or equal to the electrical polarity of the charged particles so as to minimize the deposition of the charged particles on the metal surface.
    Other aspects of the invention include coatings formed by the process described above and components protected by such coatings. The coating is well suited for protecting various types of metal surfaces from fouling, which may result from particles often contained in refrigerants, for example, in the cooling water used in boiling water nuclear reactors. Non-limiting examples are components formed of nickel-based alloys, iron-based alloys, stainless steels, for example, AISI Type 304 stainless steel, whose well-known examples are nozzles and constrictions of jet pump groups, impellers, condenser tubes, circulation pumps, and steam generator parts of boiling water nuclear reactors include.
    A noteworthy aspect of the process and the resulting coating is that the coating can be made to be dense, have a controlled thickness, and have a zeta potential on its surface that allows the coating to remove the deposits of charged particles, including radioactive species, as well as fouling substances that are normally present in cooling water. The ability to apply the coating using a colloid based process facilitates the application of the coating to components that have already been in service, in that the colloid based process of this invention does not require extensive equipment and extreme processing parameters, for example, temperatures and pressures , in comparison to other deposition processes, such as chemical vapor deposition (CVD), physical vapor deposition (PVD) and the like, and is not limited by the line of sight and other geometrical limitations, such as in CVD. In addition, the colloid based process of this invention can also provide a significant cost advantage over CVD and other typical processes normally used to deposit similar ceramic coatings.
    In one aspect, a method of forming an oxide coating comprises preparing an aqueous colloidal suspension containing from about 0.5 to about 35 weight percent nanoparticles comprising titanium oxide and / or zirconia; Depositing the aqueous colloidal suspension on a metal surface; Drying the aqueous colloidal suspension to form an unsintered coating; and heating the unsintered coating to a temperature of up to 500 ° C to densify the unsintered coating and form an oxide coating on the metal surface, the oxide coating having a zeta potential that is less than or equal to an electrical polarity of the charged particles in Contact with the oxide coating is so as to minimize the deposition of the charged particles on the metal surface.
    In another aspect, a method of preventing the deposition of charged particles on a metal surface comprises preparing an aqueous colloidal suspension containing from about 0.5 to about 35 weight percent nanoparticles containing either titanium oxide and / or zirconium oxide in water and about 0.1 to about 10% of 2- [2- (2-methoxyethoxy) ethoxy] -acetic acid (C7H14O5) or polyfluorosulfonic acid; Immersing a metal object in the aqueous colloidal suspension for a period of about 1 to about 120 minutes; Withdrawing the metal object from the aqueous colloidal suspension at a rate of about 1 to about 10 centimeters / minute; Drying the aqueous colloidal suspension to form an unsintered coating on the object; and heating the unsintered coating to a temperature of up to 500 ° C to densify the unsintered coating and form an oxide coating having a thickness of about 0.1 to about 10.0 microns and a zeta potential that is less than or equal to an electrical polarity of the charged particles in contact with the oxide coating so as to minimize the deposition of the charged particles on the metal object.
    Brief description of the drawings
    These and other features, aspects, and advantages of the present invention will become better understood when the following detailed description is read with reference to the accompanying drawings, in which like characters represent like parts throughout the drawings.<Tb> FIG. 1a, 1b and 1c <SEP> are photomicrographs of an oxide coating produced from an aqueous colloidal suspension containing about 35% by weight of titanium oxide nanoparticles and fired at a temperature of about 500 ° C.<Tb> FIG. 2a and 2b <SEP> are photomicrographs of an oxide coating formed from an aqueous colloidal suspension containing about 35% by weight titanium oxide nanoparticles and fired at a temperature of about 150 ° C.<Tb> FIG. 3a and 3b <SEP> are photomicrographs of an oxide coating formed from an aqueous colloidal suspension containing about 35% by weight titanium oxide nanoparticles and fired at a temperature of about 100 ° C.<Tb> FIG. 4a and 4b <SEP> are photomicrographs of an oxide coating formed from an aqueous colloidal suspension containing about 10% by weight titanium oxide nanoparticles and fired at a temperature of about 100 ° C.<Tb> FIG. 5a, 5b and 5c <SEP> are photomicrographs of oxide coatings produced by applying aqueous colloidal suspensions containing about 10, 20 and 35 wt% titanium oxide nanoparticles, respectively, to rotating surfaces and then heating the coatings to a temperature of about 100 ° C were generated.<Tb> FIG. Fig. 6 <SEP> schematically represents a cross-sectional view of a part of a jet pump of a type used for circulating refrigerant through a reactor pressure vessel of a boiling water nuclear reactor; and<Tb> FIG. FIG. 7 is an enlarged fragmentary cross-sectional view of a nozzle of the jet pump of FIG. 6. FIG.
    Although the above drawing figures represent alternative embodiments, other embodiments of the present invention may be contemplated, as indicated in the discussion. In all cases, this disclosure presents illustrated embodiments of the present invention by way of illustration and not limitation. Numerous other modifications and embodiments may be devised by those skilled in the art that fall within the scope and spirit of the principles of this invention.
    Detailed description of the invention
    There are many different chemical forms of "crud", for example Fe2O3, Fe3O4, NiFe2O4, Fe2Cr2O4 and the like. The most critical radioactive particle species in a nuclear reactor is Co-60, which is normally present as an ionic particle species in the reactor water body. As Co-60 deposits on the crud or oxide layer of metallic components, Co-60 reacts with additional Crud / oxide to form CoFe2O4 (radioactive Crud). The rapid diffusion of Co ions compared to all other metal ions, for example Fe, Ni, Cr and the like, readily replaces Fe, Ni or Cr and forms CoFe2O4. Since a TiO2 coating is chemically stable, the chemical reactions can be drastically reduced and the material weakens the formation of CoFe2O4 (radioactive Crud). Some other oxides or crudes, such as Fe 2 O 3 and the like, can deposit on the TiO 2 layer, but do not react kinetically with TiO 2.
    According to one aspect of the invention, the accumulation of radioactive species such as Co-60 and the like on the surfaces can be attenuated by a coating deposited on the surface of the component of interest, for example on a metal surface of a component a nuclear reactor that can come into contact with the radioactive particle types. In one embodiment, the coating is a dense oxide coating having a controlled thickness and zeta potential that is approximately identical to or less than the electrical polarity of radioactive species, for example, radioactive species present in coolants caused by boiling water -Kernreaktor flow. The coating is preferably deposited from an aqueous colloidal suspension of nanoparticles consisting of titanium oxide (TiO 2) and / or zirconium oxide (ZrO 2). The colloidal suspension is applied to the surfaces to be coated and then dried and heat treated at an elevated temperature to increase their density and adhesive strength. In order to achieve a dense oxide coating having a controlled thickness, various aspects of this process are considered individually and / or in combination to be important, such as colloidal suspension chemistry, application method, drying conditions, and heat treatment temperature. These aspects are discussed below.
    By definition, a colloid is a homogeneous, non-crystalline substance consisting of large molecules or ultramicroscopic particles of a substance dispersed in a second substance. Colloids include gels, sols and emulsions; the particles do not settle out and can not be separated by normal filtering or centrifuging, such as in a suspension. In other words, colloidal suspensions (also referred to as colloidal solution or simply colloid) are a type of chemical mixture in which one substance is uniformly distributed in the other. Particles of the dispersed substance are only dispersed in the mixture and not dissolved, as in the case of a solution. The dispersed particles in a colloid are sufficiently small that they are uniformly dispersed in the other substance (for example, a gas, liquid, or solid) to maintain a homogeneous appearance but are sufficiently large so as not to dissolve. In the present invention, the dispersed substance comprises (or contains) nanoparticles of titanium oxide and / or zirconium oxide, and is dispersed in water as a preferable dispersion medium. The dispersed nanoparticles preferably have diameters of up to about 200 nanometers, more preferably less than 150 nanometers, and most preferably in the range of 2 to 50 nanometers. The colloidal suspension may contain from about 0.5 to about 35 wt% nanoparticles, more preferably from about 5 to about 20 wt% nanoparticles. The colloidal suspension also preferably contains from about 0.1% to about 10% of 2- [2- (2-methoxyethoxy) ethoxy] -acetic acid (C7H14O5) or polyfluorosulfonic acid in water.
    Deposition of the colloidal suspension may be carried out by dipping, spraying or various other methods such as filling a cavity, although it has been shown by dipping method to provide excellent results in terms of surface morphology and control of coating thickness as well as facilitating the coating of Surfaces that otherwise would be difficult to coat by a visual line process. In preferred embodiments, the suspension is deposited by immersing the component in the suspension for a time sufficient to accumulate a suspension coating of a desired thickness. A suitable duration is from about 1 to about 120 minutes. By retracting the component from the suspension at a rate of up to 10 centimeters / minute, more preferably at a rate of about 1 to about 5 centimeters / minute, a layer of the suspension may be applied to a controlled thickness of about 0.1 to about 10 Microns, more preferably from about 0.5 to about 2.0 microns.
    The colloidal suspension layer is then air dried to yield a green coating on the component surface. The air-drying may be carried out at about room temperature (about 25 ° C) for about sixty minutes, for example, about thirty seconds to about thirty minutes, or better, about one minute to ten minutes. The unsintered coating then undergoes a heat treatment to densify the coating and achieve a completely ceramic (oxide) coating. For this purpose, the unsintered coating is preferably heated at a rate of about 1.0 to 10.0 ° C / minute and preferably about 2 to 5 ° C / minute. The temperature of the heat treatment may be up to 500 ° C, for example 100 to 500 ° C, although better below 150 ° C and most preferably in the range of 100 to 120 ° C. The temperature of the heat treatment is maintained for a period of from about 30 minutes to about 3 hours, more preferably from about 45 minutes to about 1 hour. During the heat treatment, increased strengthening and sedimentation of the nanoparticles occurs at high temperature.
    The above parameters were determined by several investigations with colloidal suspensions containing titanium oxide nanoparticles. In particular, these studies have demonstrated the importance of using relatively low concentrations of nanoparticles and relatively low heat treatments to promote surface morphology, crack resistance and adhesion of the final ceramic coatings. In particular, it has been found that lower concentrations and heat treatment temperatures improve the adhesion of the coating to levels of 10 ksi (about 70 MPa) or more and promote a crack-free and smoother coating surface which is less likely to cause physical adhesion of radioactive species and fouling agents in the cooling water promotes a boiling water nuclear reactor.
    In a first series of studies, titanium oxide coatings were deposited on the honed surfaces of Type 304 stainless steel samples. The titanium oxide coatings were formed either from aqueous colloidal suspensions containing about 35% by weight titanium oxide nanoparticles or from sol-gel solutions containing titanium isopropoxide as the titanium oxide precursor. Several samples made of each type of coating concluded that smooth, dense and adherent titanium oxide coatings were much easier to achieve with colloidal suspensions than with sol-gel solutions.
    In a second series of investigations, various colloidal suspensions were prepared from a colloidal suspension containing about 35% by weight of titanium oxide nanoparticles in water, with a reported particle size of less than 150 nanometers. From this solution, diluted colloidal suspensions containing 20% by weight or 10% by weight of titanium oxide nanoparticles were prepared. Test samples for this first set of tests were Type 304 stainless steel samples, the surfaces of which were precision ground prior to coating.
    Titanium oxide coatings were applied to a first group of samples by immersing the samples in the 35% colloidal suspension for about 30 minutes, withdrawing the samples at a rate of about 1.0 centimeters / minute, air drying for about 5 minutes, and then heating the resulting unsintered coatings at a temperature of about 500 ° C over a period of about 60 minutes. The resulting ceramic coatings had thicknesses of about 0.5 to about 1.0 microns. Figures 1a and 1b are microphotographs of the surface of one of the coatings taken at magnifications of 10 kx and 50 kx respectively, and Figure 1c is a microfoto showing a cross section of the sample at an enlargement of 20 kx. An adhesion test carried out on the sample showed that the coating had an adhesive strength of about 11.3 ksi (about 78 MPa).
    Titania coatings were applied to a second group of samples by immersing the samples in the 35% colloidal suspension for about 30 minutes, withdrawing the samples at a rate of about 1.0 centimeters / minute, air drying the coatings for about 5 minutes Minutes and then heating the coatings at a temperature of about 150 ° C over a period of about 60 minutes. The resulting coatings had thicknesses of about 0.5 to about 1.0 microns. Figures 2a and 2b are photomicrographs of the surface and cross-section of one of the coatings taken at magnifications of 5 kx and 25 kx, respectively. The relatively low temperature (150 ° C) compared to 500 ° C still gave acceptable coating properties. An adhesion test carried out on the sample showed that the coating had an adhesive strength of about 9.8 ksi (about 67 MPa).
    Titanium oxide coatings were applied to a third group of samples by immersing the samples in the 35% colloidal suspension for about 30 minutes, withdrawing the samples at a rate of about 1.0 centimeter / minute, air-drying the coatings for about 5 minutes Minutes and then heating the coatings at a temperature of about 100 ° C over a period of about 60 minutes. The resulting coatings had thicknesses of about 0.5 to about 1.0 microns. Figures 3a and 3b are photomicrographs of the surface and cross-section of one of the coatings taken at magnifications of 5 kx. The relatively low temperature (100 ° C compared to 500 ° C) still gave acceptable coating properties. An adhesion test carried out on the sample showed that the coating had an adhesive strength of about 11.6 ksi (about 80 MPa).
    Titania coatings were applied to a fourth group of samples by immersing the samples in the 10% colloidal suspension for about 30 minutes, drawing the samples out at a rate of about 1.0 centimeter / minute, air-drying the coatings for about 5 minutes Minutes and then heating the coatings at a temperature of about 100 ° C over a period of about 60 minutes. The resulting coatings had thicknesses of about 0.5 to about 1.0 microns. Figures 4a and 4b are photomicrographs of the surface and cross-section of one of the coatings taken at magnifications of 5 kx and 50 kx, respectively. The relatively low colloidal percentage (10% vs. 35%) still provided acceptable coating properties. An adhesion test carried out on the sample showed that the coating had an adhesive strength of about 11.5 ksi (about 79 MPa).
    A third series of studies was set up to further study heat treatments at 100 ° C carried out on titanium oxide coatings formed from aqueous colloidal suspensions containing 10, 20 or 35% by weight titanium oxide nanoparticles , The particle size of the titanium oxide nanoparticles was about 30 to 40 nanometers. Test specimens for this series of tests were 304SS pipes that were about 0.75 inches (about 19 mm) in diameter and whose inner surfaces were finish ground before coating.
    Titanium oxide coatings were formed on a first group of 304SS tubes by rotating the tubes at a speed of about 125 rpm while distributing either the 10%, 20% or 35% colloidal suspension inside the tube has been. The tubes were rotated for about 30 minutes, after which the resulting colloidal coatings were air dried for about 5 minutes and then fired at a temperature of about 100 ° C over a period of 1 hour. The resulting oxide coatings had thicknesses of about 0.5 to about 1.0 microns. Figures 5a, 5b and 5c are photomicrographs of the surfaces of coatings formed from 10%, 20% and 35% colloidal coatings, respectively.
    As mentioned above, components exposed to aqueous high temperature environments, for example nozzles and throat areas of jet pump assemblies, impellers, condenser tubes, recirculation pumps and steam generator parts in boiling water nuclear reactors, are exposed to fouling resulting from charged particles in the hot coolant ( normally water from about 100 to about 300 ° C) which deposit on metal surfaces of the components. Over time, fouling results in the formation of a thick, dense oxide "crud" layer on the exposed surfaces of the component. The accumulation of fouling agents is a difficult operating and maintenance problem for, for example, boiling water nuclear reactors, because the accumulation of fouling agents substantially improves the efficiency of the coolant recirculation system of a reactor by reducing flow rates of the coolant (water) and reducing the performance of the cooling system decreases. The process of the invention forms an oxide coating on a metal surface to reduce the deposition of charged particles on the metal surface when contacted with a coolant containing the charged particles.
    Fig. 6 schematically illustrates a portion of a jet pump 10 of a type used in a boiling water nuclear reactor coolant recirculation system as an example of an application of the coating of the invention to reduce the accumulation of radioactive species on a metal surface , The jet pump 10 may be one of a plurality of jet pumps normally located in an annular space between a wall of a reactor pressure vessel and a core shell of the reactor. The annular space contains coolant which is circulated by the jet pumps around the nuclear reactor jacket. The jet pump 10 is shown in FIG. 6 as including an inlet riser 12 (shown as a phantom) through which coolant is withdrawn from a suitable source, for example a recirculation pump, which draws coolant from the annular space. The riser 12 is shown connected via a knee 14 to a mixer group comprising a mixer 16 below a nozzle group 18. A diffuser group 20 is located on the discharge side of the mixer 16 and directs the refrigerant, for example, to a lower core collector of the reactor for delivery to the fuel rods of the reactor. Although a single mixer group is shown in FIG. 6, an inlet riser 12 may be connected to a pair of mixer groups, the second mixer group being similarly configured and located on the opposite side of the riser 12.
    As can be seen in Figures 6 and 7, the nozzle assembly 18 has a plurality of nozzles 22, each defining an aperture 24 (Figure 7). The walls of the nozzles 22 defining the openings 24 are normally frusto-conical in shape with the diameters decreasing in the direction of the coolant flow to increase the flow rate of the coolant in the mixer 16. The internal passageway through the mixer 16 generally has a constant cross-sectional shape and size. The surfaces of the mixer 16 and the nozzles 22 which come into contact with the coolant are normally formed of a stainless steel, a notable, but non-limiting example being AISI type 304, although it is understood that these components are made of other materials including other iron-based alloys and nickel-based alloys. Other details and aspects of jet pump 10 and recirculation systems in which it can be installed are well known in the art and therefore will not be discussed in further detail herein.
    As a result of the coolant being pumped by the recirculation pump, the coolant flows up through the riser 12, through the elbow 14, and then down through the nozzle assembly 18 and its openings 24 into the mixer 16. Accelerate the orifices 24 the coolant flow into the mixer 16 and the removal of coolant from the surrounding annular space in the mixer 16 through an annular inlet 26 surrounding the nozzle group 18, which causes mixing of the accelerated refrigerant with the refrigerant which is withdrawn from the annular space , The coolant, usually at temperatures of about 250 to about 350 ° C, is constantly circulated through the jet pump 10, with the result that the jet pump 10 (and other components of the recirculation system) is subject to fouling, which is charged particles within hot Coolant (usually water) results, which tend to deposit on the surfaces of the components, and in particular on the surfaces which define the inner coolant passages of the mixer 16 and the nozzles 22. The accumulation of such deposits eventually leads to fouling, generally in the formation of a thick, dense oxide "crud" layer on the component surfaces, causing operational and maintenance problems as a result of the deterioration in the efficiency of the coolant flow. The coating of the invention reduces or eliminates the accumulation of "crud" containing radioactive species on components exposed to high temperature water environments, for example nozzles and constrictions of jet pump assemblies, impellers, condenser tubes, recirculation pumps and steam generator parts in boiling water nuclear reactors.
    Although the invention has been described in terms of a preferred embodiment, it will be appreciated that other forms may be adopted by those skilled in the art. Therefore, the scope of the invention should be limited only by the following claims.
    权利要求:
    Claims (10)
    [1]
    A method of forming an oxide coating, comprising:Depositing an aqueous colloidal suspension containing 0.5 to 35% by weight of nanoparticles comprising either titanium oxide or zirconium oxide on a metal surface;Drying the aqueous colloidal suspension to form an unsintered coating; andHeating the unsintered coating to a temperature of up to 500 ° C to densify the unsintered coating and form an oxide coating on the metal surface;wherein the oxide coating has a zeta potential that is less than or equal to an electrical polarity of the charged species of particles in contact with the oxide coating so as to minimize the deposition of the charged particles on the metal surface.
    [2]
    2. The method of claim 1, wherein the nanoparticles have a diameter of up to 200 nanometers.
    [3]
    The process of claim 1 wherein the aqueous colloidal suspension further contains from 0.1% to 10% of 2- [2- (2-methoxyethoxy) ethoxy] -acetic acid, C7H14O5, or polyfluorosulfonic acid in water.
    [4]
    4. The method of claim 1, wherein the aqueous colloidal suspension is deposited by immersing the metal surface in the aqueous colloidal suspension for a period of 1 minute to 120 minutes and at a temperature of 25 to 35 ° C.
    [5]
    The method of claim 1, wherein the metal surface is withdrawn from the aqueous colloidal suspension at a rate of 1.0 to 10.0 centimeters / minute.
    [6]
    6. The method of claim 1, wherein the aqueous colloidal suspension is air dried at a temperature of 25 ° C to 35 ° C for a period of 5 minutes to 60 minutes.
    [7]
    The method of claim 1, wherein the unsintered coating is heated to a temperature of from 100 ° C to 500 ° C for a period of from 30 minutes to 3 hours.
    [8]
    The method of claim 1, wherein the unsintered coating is heated at a rate of 1.0 ° C / min to 10.0 ° C / min.
    [9]
    The method of claim 1, wherein the oxide coating has an adhesive strength of at least 70 MPa on the metal surface.
    [10]
    10. oxide coating formed by the method according to claim 1.
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    法律状态:
    2017-03-15| NV| New agent|Representative=s name: GENERAL ELECTRIC TECHNOLOGY GMBH GLOBAL PATENT, CH |
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