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WO2012002176A1 - Procédé de durcissement de surface d'article moulé en platine et article moulé en platine présentant une surface durcie - Google Patents

Procédé de durcissement de surface d'article moulé en platine et article moulé en platine présentant une surface durcie Download PDF

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Publication number
WO2012002176A1
WO2012002176A1 PCT/JP2011/063924 JP2011063924W WO2012002176A1 WO 2012002176 A1 WO2012002176 A1 WO 2012002176A1 JP 2011063924 W JP2011063924 W JP 2011063924W WO 2012002176 A1 WO2012002176 A1 WO 2012002176A1
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WIPO (PCT)
Prior art keywords
platinum
coating
coating layer
molded product
iridium
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Ceased
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PCT/JP2011/063924
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English (en)
Japanese (ja)
Inventor
島宗　孝之
重治 赤塚
松下　桂一郎
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Furuya Metal Co Ltd
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Furuya Metal Co Ltd
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Publication of WO2012002176A1 publication Critical patent/WO2012002176A1/fr
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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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00—Aeronautics or air transport
    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft

Definitions

  • the present invention relates to a method for curing the surface of a platinum molded article and a platinum molded article having a cured surface.
  • the single crystal synthesized using the pressure vessel is, for example, artificial quartz or zinc oxide in the hydrothermal synthesis method, and is, for example, gallium nitride in the low temperature synthesis method. These single crystals are used for various applications such as optics and electronic elements, and high purity is required. Therefore, the inner surface of the pressure vessel is required not to elute impurities in an ultra-high temperature and ultra-high pressure state, and is generally formed of platinum or a platinum alloy having excellent corrosion resistance and durability.
  • the molded product is used in a wide variety of fields such as physics and chemistry experiments at high temperature conditions and mining industry.
  • platinum is easily deformed due to its softness.
  • the specific gravity is large, if the thickness of the molded product is thin, it may be deformed by its own weight. Therefore, in order to maintain strength, it is necessary to increase the thickness of the molded product.
  • the amount of platinum used increases, there is a problem that the material price naturally increases and the molded product becomes very expensive. It was.
  • the pressure vessel usually has a double structure in which the physical strength is held by an outer cylinder made of a nickel-base alloy, and a thin molded product formed of platinum for the purpose of corrosion resistance is used as the inner cylinder container.
  • an outer cylinder made of a nickel-base alloy
  • a thin molded product formed of platinum for the purpose of corrosion resistance is used as the inner cylinder container.
  • Platinum has the property of being heat resistant and chemically stable, but has the property of easily causing grain growth and intergranular corrosion in a high temperature reducing atmosphere. Therefore, when used as an inner cylinder of a pressure vessel that is exposed to a high-temperature reducing atmosphere such as a low temperature synthesis method, there is a problem that platinum is consumed quickly and the life of the inner cylinder is shortened. On the other hand, iridium and ruthenium are known to be stable against a high-temperature reducing atmosphere.
  • Platinum alloys are known to have better physical strength and chemical stability than platinum. However, when platinum is used as an alloy, there is a problem that workability is extremely inferior. There are almost no cases where these alloys are used as the inner cylinder of a pressure vessel. Further, as shown in paragraphs 0034 and 0035 of Patent Document 2, the pressure vessel is easily deformed in order to prevent the inner tube vessel from being deformed or damaged due to the difference between the internal pressure and the external pressure. However, it is preferable to install a pressure buffering mechanism such as a bellows structure for eliminating the pressure difference, but platinum alloys cannot be used for bellows because of their poor workability. Therefore, even if an alloy of platinum is used for the inner cylinder container, platinum is used for the bellows, which has a problem that the structure becomes complicated.
  • Patent Document 3 proposes a technique for chemically and physically stabilizing the surface of a titanium base material by applying a precious metal coating to the surface of the titanium base material. This is a technology that forms a titanium layer and coats the electrode material containing noble metal on its surface, improving the strength of the platinum molded product, and preventing platinum from causing grain growth and intergranular corrosion in a reducing atmosphere. Not to do.
  • the object is to provide a platinum molded article having a cured surface and a surface hardening method thereof, which can prevent growth and intergranular corrosion.
  • the platinum molding surface hardening method includes a coating step of coating a coating liquid containing either or both of an iridium salt and a ruthenium salt on the surface of the platinum molding, And pyrolyzing the coating layer in a nitrogen gas atmosphere or in a flame to form the coating layer as a coating layer made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium. .
  • the surface-curing method for a platinum molded product according to the present invention is more suitable for a form in which the thickness of the platinum molded product is 0.2 to 1.0 mm (0.2 mm to 1.0 mm). Even if the platinum molded product is thin, the strength can be maintained.
  • the method for surface hardening a platinum molded product according to the present invention it is preferable that the method further includes a step of nitriding a partial region or the entire region of the surface of the coating layer.
  • the surface of the platinum molded product can be made harder.
  • oxide formation can be prevented, and a product with higher purity can be obtained in the low-temperature synthesis method.
  • the coating solution preferably further contains a platinum compound.
  • the coating layer can be an alloy of either iridium or ruthenium or both and platinum, and the adhesion between the coating layer and the platinum molded product can be further enhanced.
  • the coating liquid further contains an alcohol. Since thermal decomposition becomes a reducing atmosphere and oxygen can be removed, generation of oxides can be prevented. Further, since iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium having high corrosion resistance can be precipitated more stably, corrosion can be minimized when used in a high-temperature reducing atmosphere.
  • the platinum molded product is an inner cylinder of a pressure vessel, and the application step is performed by applying the application to one or both of the inner surface and the outer surface of the inner cylinder.
  • a mode in which a liquid is applied to form the coating layer is included. Since the self-weight deformation resistance is obtained, the handleability of the inner cylinder alone is improved, and the inner cylinder can be easily attached to the pressure vessel body. In addition, in the low temperature synthesis method, platinum grain growth and intergranular corrosion can be prevented.
  • the platinum molded product is an inner cylinder of a pressure vessel, and further includes an installation process of installing the inner cylinder in the main body of the pressure vessel, the installation process
  • the coating step and the thermal decomposition step are included, and the coating step applies the coating liquid to the inner surface of the inner cylinder to form the coating layer, and the thermal decomposition step includes the coating step.
  • the inner surface of the inner cylinder can be hardened without special equipment such as a large heating furnace while being installed in the main body of the pressure vessel.
  • the platinum molded product is a shelf for attaching a seed crystal housed in a main body of a pressure vessel, and the coating step is performed on the entire surface of the shelf.
  • coating is included. Impurities can be reduced in the growth of single crystals by the low-temperature synthesis method.
  • the platinum molded product is a flange provided at an opening of a pressure vessel, and the coating step is performed on the surface of at least a portion to be a seal portion of the flange.
  • coats a coating liquid and forms the said coating layer is included.
  • the surface hardness of the flange can be increased. Further, the surface of the flange can be hardened without special equipment such as a large heating furnace while being installed in the main body of the pressure vessel.
  • the platinum molded product is a crucible, and the coating step is performed by applying the coating liquid to either or both of the inner surface and the outer surface of the crucible.
  • the form which forms the said application layer is included. Even if the crucible is thin, the handleability can be improved. Further, durability in a reducing atmosphere is improved.
  • the platinum molded product having a cured surface according to the present invention is characterized in that a coating layer made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium is provided on the surface of the platinum molded product.
  • the surface of the platinum molded product is either the inner surface or the outer surface of the inner tube of the pressure vessel, or both, or a seed crystal accommodated in the main body of the pressure vessel. It includes a form that is the entire surface of the mounting shelf, the surface of at least the portion of the flange provided at the opening of the pressure vessel, or the inner surface or the outer surface of the crucible, or both.
  • the platinum molded product having a cured surface according to the present invention includes a form in which the thickness of the platinum molded product is 0.2 to 1.0 mm. Even if the molded product is thin, it can maintain strength and has resistance to self-weight deformation.
  • the coating layer preferably has a thickness of 1 to 30 ⁇ m.
  • the surface of the platinum molding can be coated to improve chemical stability and physical strength.
  • the platinum element of the platinum molded product and the metal element contained in the coating layer are diffused. Adhesion between the platinum molded product and the coating layer is improved, and chemical stability and physical strength can be further improved.
  • the platinum molded product having a cured surface In the platinum molded product having a cured surface according to the present invention, nitriding treatment of an alloy containing at least one kind of iridium, ruthenium, iridium or ruthenium on at least the surface side of the coating layer in a partial region or the entire region of the coating layer. A layer is preferred.
  • the surface of the platinum molded product can be made harder. In addition, oxide formation can be prevented, and a product with higher purity can be obtained in the low-temperature synthesis method.
  • the thickness of the nitriding layer is preferably 1 to 30 ⁇ m.
  • the surface of the platinum molded product can be made harder.
  • the present invention is excellent in its own weight deformation resistance even if it is thin, is not easily deformed, is easy to handle, has corrosion resistance and durability in a high temperature and high pressure state, and grows platinum particles in a reducing atmosphere. It is possible to provide a platinum molded article having a cured surface capable of preventing intergranular corrosion and a method for curing the surface.
  • FIG. 4 It is a schematic diagram which shows one form of the cross-sectional structure of the platinum molded product which concerns on this embodiment. It is sectional drawing which shows an example of the pressure vessel which has a shelf. It is sectional drawing which shows an example of the pressure vessel which has an inner cylinder container. It is sectional drawing which shows an example of a large sized pressure vessel. It is the elements on larger scale which show the seal part of the pressure vessel shown in FIG. 4, (a) is a section fragmentary enlarged view which shows one form of a flange and a gasket, (b) is a top view which shows one form of a gasket. is there.
  • FIG. 1 is a schematic diagram showing an embodiment of a cross-sectional structure of a platinum molded product according to this embodiment.
  • the platinum molded product 100 having a hardened surface according to this embodiment is provided with a coating layer 30 made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium on the surface of the platinum molded product 20.
  • the type of the platinum molded product 20 is not particularly limited.
  • a seed crystal mounting shelf (baffle / saddle / crystal mounting) housed in the inner body of the pressure vessel or the main body of the pressure vessel (hereinafter referred to as a shelf).
  • a flange and a crucible provided at the opening of the pressure vessel.
  • the inner cylinder of the pressure vessel forms a sealed space by itself, is accommodated in the main body of the pressure vessel and is used without being joined to the pressure vessel (hereinafter referred to as an inner cylinder container) and pressure.
  • It includes a lining-type inner cylinder (hereinafter referred to as an inner cylinder) that is housed in a container body and used in close contact with or adhered to the inner surface of the pressure vessel body.
  • the thickness of the platinum molded product 20 is preferably 0.2 to 1.0 mm. More preferably, it is 0.3 to 0.7 mm. If it is less than 0.2 mm, it may be inferior to physical strength and resistance to self-deformation. If the thickness exceeds 1.0 mm, it is difficult to reduce the price of the molded product by making the platinum molded product thinner and reducing the amount of platinum used.
  • the thickness of the platinum molded product 20 may be uniform as a whole, or the thickness may be partially changed.
  • the form in which the thickness is partially changed is, for example, a form in which the inner cylinder is reinforced by making the thickness of the flange and the thickness of the bottom thicker than the thickness of the cylinder. At this time, it is preferable that the thickness of the thinnest part (for example, the thickness of the side wall part or the bottom part of the cylinder) is 0.2 to 1.0 mm.
  • the covering layer 30 is made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium.
  • An alloy containing iridium, ruthenium, or at least one of iridium or ruthenium has a property of hardly causing grain growth in a reducing atmosphere. Moreover, since those melting
  • the platinum molded product 100 with the surface cured according to the present embodiment is exposed to iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium on the surface, so that chemical stability in a reducing atmosphere is achieved. Can be improved.
  • iridium alloys examples include iridium-ruthenium alloys, iridium-platinum alloys, iridium-rhodium alloys, iridium-gold alloys, and iridium-rhenium alloys.
  • the alloy containing ruthenium examples include a ruthenium-iridium alloy, a ruthenium-platinum alloy, a ruthenium-rhodium alloy, a ruthenium-gold alloy, and a ruthenium-rhenium alloy.
  • an iridium-platinum alloy or ruthenium-platinum alloy which is an alloy with platinum, is preferable in that the adhesion to the platinum molded product 20 is further improved and the physical strength and the chemical stability are further improved.
  • the platinum content is preferably 10 to 70% by mass, more preferably 15 to 60% by mass. If the platinum content in the alloy is less than 10% by mass, the desired effect may not be obtained. When it exceeds 70 mass%, physical strength and corrosion resistance in a reducing atmosphere may be insufficient. In particular, sufficient hardness may not be obtained and the intended purpose may not be achieved.
  • the coating layer 30 does not contain the oxide of iridium or ruthenium. A reaction product with higher purity can be obtained.
  • the metal contained in the coating layer 30 is iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium can be appropriately selected according to the conditions and purpose of use.
  • an alloy is not limited to the alloy which consists of 2 types of illustrated metals, As long as it alloyes, it can be set as the alloy which consists of 3 or more types of metals.
  • the alloys composed of three or more metals include, for example, ruthenium-platinum-rhodium alloy, iridium-platinum-rhodium alloy, iridium-ruthenium-rhodium alloy, iridium-platinum-rhenium alloy, ruthenium-platinum-rhenium alloy, iridium-ruthenium.
  • the platinum element of the platinum molded product 20 and the metal elements such as iridium and ruthenium contained in the coating layer 30 are diffused.
  • the platinum of the platinum molded product 20 and the coating layer 30 of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium are diffused so that the platinum molded product 20 and the coating layer 30 are integrated to improve adhesion. , Physical strength and chemical stability can be further improved.
  • the diffusion state includes, for example, a state in which platinum element diffuses from the platinum molded product 20 into the coating layer 30, a state in which a metal element diffuses from the coating layer 30 into the platinum molded product 20, and a platinum element from the platinum molded product 20 into the coating layer 30. It is an interdiffusion state in which the metal element diffuses and the metal element diffuses from the coating layer 30 into the platinum molded product 20.
  • the platinum molded article 100 having a hardened surface forms a coating layer made of iridium, ruthenium, or an alloy containing at least one kind of iridium or ruthenium after molding platinum having good workability.
  • the interface between the platinum molded product 20 and the coating layer 30 is alloyed.
  • physical strength and chemical stability can be increased. Therefore, it can respond to the platinum molded product 20 of various shapes.
  • the covering layer 30 may be formed of only one layer, or may be formed of two or more layers. In the case of forming with two or more layers, the configuration of each layer can be changed.
  • the first coating layer adjacent to the platinum molded product 20 is preferably a layer made of an alloy of platinum and at least one kind of iridium or ruthenium.
  • the first coating layer and the second coating layer are sequentially provided on the surface of the platinum molded product 20, for example, the first coating layer is made of iridium or an alloy of ruthenium and platinum, and the second coating layer is made of iridium or ruthenium. And rhodium alloy.
  • the second coating layer may contain a third metal in addition to iridium and ruthenium, or iridium and ruthenium.
  • a third metal in addition to iridium and ruthenium, or iridium and ruthenium.
  • the structure of each layer is iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium can be selected as appropriate according to the use conditions and purpose, and the present embodiment is not limited to this.
  • the metal elements contained in each coating layer formed of two or more layers are diffused in the same manner as the platinum element of the platinum molded product 20 and the metal contained in the coating layer 30. Since each layer is united and alloyed by diffusion, adhesion is improved, and physical strength and chemical stability can be enhanced.
  • the thickness of the coating layer 30 is preferably 1 to 30 ⁇ m. More preferably, it is 3 to 10 ⁇ m. If it is less than 1 ⁇ m, physical strength and corrosion resistance in a reducing atmosphere may be insufficient. In some cases, the coating layer 30 may be buried by diffusion of the platinum molded product 20 with the platinum element. If it exceeds 30 ⁇ m, the coating layer 30 is likely to peel off depending on handling conditions such as rapid heating and quenching due to the difference in thermal expansion coefficient between the platinum element of the platinum molded product 20 and the metal contained in the coating layer 30. In addition, the amount of metal used such as iridium and ruthenium increases, which is not economically preferable. When the covering layer 30 is formed of two or more layers, the total thickness of all the covering layers is within the above range. Moreover, thickness can be changed for every layer.
  • An alloy containing at least one kind of iridium, ruthenium, or iridium or ruthenium has a characteristic of absorbing oxygen, albeit slightly. Therefore, in the case of being used for a reaction in a reducing atmosphere such as a low-temperature synthesis method, there is an effect that the reducing atmosphere can be maintained.
  • the platinum molded product 100 having a hardened surface includes iridium, ruthenium, or at least one kind of iridium or ruthenium.
  • the nitriding layer (not shown) is preferable.
  • the surface of the platinum molded product 100 can be further cured.
  • a reaction such as a low-temperature synthesis method is used as a reaction in which oxygen becomes an impurity. It is suitable for use.
  • the platinum molded product 20 when a partial region of the coating layer 30 is a nitriding layer, for example, it becomes a seal portion that requires particularly physical strength. Only the portion is a nitriding layer.
  • a partial region of the coating layer 30 when a partial region of the coating layer 30 is a nitriding layer, for example, a part of the inner surface that requires corrosion resistance, and a part in contact with a chemical used for the reaction can be in contact. Only the portion is a nitriding layer.
  • the nitriding layer contains iridium, ruthenium, or an alloy nitride containing at least one of iridium or ruthenium contained in the coating layer 30.
  • the nitride content of the nitriding layer has a distribution in which the surface is the largest and gradually decreases toward the inside of the substrate.
  • the thickness of the nitriding layer is preferably 1 to 30 ⁇ m. More preferably, it is 1 to 10 ⁇ m. If it is less than 1 ⁇ m, the effect of curing the surface may be insufficient.
  • the surface of the nitriding layer becomes brittle, the surface becomes brittle due to the occurrence of cracks due to residual stress inside the nitriding layer, and peeling may occur when pressure is applied.
  • the time required for the nitriding treatment becomes long, it is not economically preferable.
  • the platinum molding surface hardening method includes a coating step in which a coating liquid containing one or both of an iridium salt and a ruthenium salt is applied to the surface of the platinum molding 20 to form a coating layer. And a thermal decomposition step of thermally decomposing the coating layer in a nitrogen gas atmosphere or flame to form the coating layer 30 made of iridium, ruthenium, or an alloy containing at least one kind of iridium or ruthenium.
  • the platinum molded product 20 can be obtained by a generally known method such as a casting method, a forging method, press molding, welding, or the like. Therefore, the method for molding the platinum molded product 20 is not particularly limited in the present embodiment.
  • the thickness of the platinum molded product 20 is preferably 0.2 to 1.0 mm.
  • a coating solution containing either or both of an iridium salt and a ruthenium salt is coated on the surface of the platinum molded product 20 and dried to form a coating layer.
  • the coating solution is not particularly limited in the present embodiment as long as it can form the coating layer 30 by depositing iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium by thermal decomposition performed later.
  • the coating solution is, for example, a solution in which an iridium salt or a ruthenium salt is mixed with alcohol as a solvent.
  • the iridium salt include iridium chloride, iridium nitrate, chloroiridic acid, and iridium butoxide.
  • the ruthenium salt examples include ruthenium chloride, ruthenium nitrate, ruthenium chloride, and ruthenium butoxide.
  • the iridium salt is preferably iridium chloride in that it can efficiently precipitate iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium by thermal decomposition.
  • the ruthenium salt is preferably ruthenium chloride because it is easily available and relatively inexpensive.
  • the coating liquid may further contain a metal compound that forms an alloy with iridium or ruthenium.
  • metal compounds forming alloys with iridium or ruthenium include platinum compounds such as chloroplatinic acid and dinitrodiammine platinum, rhodium compounds such as rhodium chloride and rhodium nitrate, gold compounds such as chloroauric acid, gold chloride and gold cyanide.
  • Compounds, rhenium compounds such as rhenium chloride and rhenium nitrate.
  • chloroplatinic acid, dinitrodiammine platinum and the like are preferably used as the platinum compound, and chloroplatinic acid is particularly preferred for combination with iridium salts and ruthenium salts. Since an alloy of iridium or ruthenium and platinum is formed and adhesion to the platinum molded article is increased, physical strength and corrosion resistance in a reducing atmosphere are further improved.
  • the coating solution preferably contains alcohol as a solvent.
  • alcohol is a solvent and an organic reducing agent.
  • examples of the alcohol include methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, isobutanol, tert-butanol, and 1-pentanol.
  • the coating solution may further contain an organic reducing agent other than alcohol such as turpentine oil.
  • the present embodiment is not limited to the method of applying the coating liquid and the method of drying.
  • the coating layer is thermally decomposed in a nitrogen gas atmosphere or in a flame, whereby one or both of iridium salt and ruthenium salt and iridium or ruthenium and alloy contained in the coating layer obtained in the coating step are alloyed.
  • the coating layer 30 is formed by precipitating a metal compound that forms iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium. When iridium and ruthenium are thermally decomposed in an atmosphere containing oxygen, an oxide is formed. Therefore, the metal can be precipitated by thermally decomposing the coating layer in a nitrogen gas atmosphere or in a flame.
  • Pyrolysis is preferably performed in a nitrogen atmosphere using a heating furnace capable of supplying nitrogen gas.
  • a heating furnace capable of supplying nitrogen gas.
  • thermal decomposition can be performed in a flame using a gas burner in an atmospheric atmosphere.
  • oxygen in the air is used for combustion, the surface of the platinum molded product is substantially in a nitrogen atmosphere, and can deposit iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium as a metal.
  • the coating liquid contain alcohol, a reducing atmosphere can be obtained and generation of oxides can be prevented.
  • the thickness of the coating layer 30 is preferably 1 to 30 ⁇ m. More preferably, it is 1 to 10 ⁇ m. It is preferable to repeat the coating step and the thermal decomposition step a plurality of times until the thickness is reached. A uniform coating layer with few pores can be obtained, and the surface of the platinum molded product can be more reliably covered with iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium.
  • the coating amount per coating step is preferably 0.05 to 1 ⁇ m. More preferably, it is 0.10 to 0.5 ⁇ m.
  • the components of the coating solution may be the same in all coating steps, or two or more types of coating solutions may be used.
  • the coating solution used in the first coating step may contain a platinum compound such as chloroplatinic acid in addition to one or both of the iridium salt and the ruthenium salt. preferable.
  • the coating solution is applied as an alcohol solution of iridium chloride and chloroplatinic acid once.
  • the coating solution is an alcohol solution of iridium chloride and ruthenium chloride, and the coating amount per coating step is 0.4 ⁇ m. .
  • a two-layer coating layer comprising a first coating layer made of iridium-platinum alloy formed on the surface of the platinum molded product 20 and a second coating layer made of iridium formed on the first coating layer. 30 can be formed. Since the coating layer 30 has improved adhesion to the platinum molded product 20, physical strength and corrosion resistance in a reducing atmosphere are further improved. Furthermore, since the coefficient of thermal expansion (linear expansion coefficient) occurs in stages, the coating layer itself is less likely to break during heating and cooling, and is difficult to peel off.
  • diffusion is performed between the platinum element of the platinum molded product 20 and the metal element contained in the coating layer 30.
  • the diffusion may be performed simultaneously with the thermal decomposition process by heating in the thermal decomposition step, but after the thermal decomposition step, further heating is performed to diffuse the platinum element of the platinum molded product 20 and the metal element contained in the coating layer 30.
  • a metal containing at least one kind of iridium or ruthenium is pre-alloyed to form a coating layer in the pyrolysis step, By further heating in the stabilization step, diffusion can be performed more efficiently.
  • the coating layer is formed by repeating the coating step and the thermal decomposition step a plurality of times, in the thermal decomposition step, a metal containing at least one kind of iridium or ruthenium is alloyed in the thermal decomposition step, and the stabilization step is performed. Diffusion treatment can be performed between the metals contained in the adjacent coating layers and between the platinum element of the platinum molded product and the metal contained in the first coating layer adjacent to the platinum molded product.
  • the heating conditions are not particularly limited.
  • the heating temperature is set to 700 to 1000 ° C. and the heating time is set to 1 to 2 hours, so that the thermal decomposition process and the diffusion process can be performed simultaneously.
  • the heating temperature is set to 500 to 600 ° C.
  • the processing time is set to 5 to 15 minutes, and the thermal decomposition process is performed.
  • the heating temperature is set to 700
  • the diffusion treatment is performed at a temperature of ⁇ 1000 ° C. and a heating time of 1 to 2 hours.
  • the diffusion treatment can be performed in an inert atmosphere such as nitrogen or argon or in an oxygen-containing atmosphere such as air. More preferably, it is in an inert atmosphere such as nitrogen or argon.
  • an inert atmosphere such as nitrogen or argon.
  • the method for hardening a surface of a platinum molded article according to the present embodiment further includes a step of nitriding a partial region or the entire region of the surface of the coating layer 30.
  • the nitriding treatment can be performed by heating in a gas containing nitrogen or a nitrogen compound.
  • the gas containing nitrogen or a nitrogen compound is not particularly limited, and examples thereof include nitrogen gas, ammonia gas, and nitrogen-hydrogen mixed gas.
  • the heating temperature and the heating time are not particularly limited, and it is preferable to select conditions under which the thickness of the nitriding layer is in the range of 1 to 30 ⁇ m, for example. By nitriding, the surface hardness of the platinum molded product can be further increased.
  • a method of nitriding a part of the region is not particularly limited, and for example, there is a method of masking a portion where nitriding is not performed.
  • FIG. 2 is a cross-sectional view showing an example of a pressure vessel having a shelf.
  • a pressure vessel 119 shown in FIG. 2 is used as a single crystal growth vessel.
  • the basic configuration of the pressure vessel 119 is as follows.
  • the pressure vessel 119 has a main body 1 and a lid 2.
  • the main body 1 and the lid 2 are made of a heat-resistant alloy such as low alloy steel or nickel chrome alloy, for example.
  • the main body 1 is heated by a heater 4 disposed on the outer periphery thereof.
  • a lower inner cylinder 105 is installed inside the main body 1.
  • the lower inner cylinder 105 is formed with a flange 105a (hereinafter also referred to as a lower flange).
  • an upper inner cylinder 106 is installed in the inside of the lid 2 in the same manner as the main body 1.
  • the upper inner cylinder 106 is formed with a flange 106a (hereinafter also referred to as an upper flange).
  • the lower inner cylinder 105 and the upper inner cylinder 106 are lining type inner cylinders.
  • the main body 1 has a bottomed cylindrical shape with one end opened, and a lower flange 105a projecting in the centrifugal direction is provided on the outer peripheral edge of the opening.
  • the pressure vessel 119 is structured to be sealed by being fixed with a fixing tool 3 such as a nut or a clamp through a gasket 7 between the upper flange 106a and the lower flange 105a.
  • the contact portion is referred to as a seal portion.
  • a seal portion a seal portion
  • the lower inner cylinder 105 and the upper inner cylinder 106 are formed of a metal having heat and corrosion resistance such as platinum.
  • the gasket 7 is formed of a metal having heat and corrosion resistance, such as a nickel-based alloy or a platinum group metal, and more preferably formed of a material having lower hardness than the upper flange 106a and the lower flange 105a.
  • a shelf 108 is accommodated in the main body 1 of the pressure vessel 119 shown in FIG.
  • the shelf 108 is a platinum frame.
  • the shelf 108 has a seed crystal gantry 10 at the upper part, a raw material 11 at the lower part, and a convection control plate 9 between the seed crystal gantry 10 and the raw material 11, and is filled with a solvent (not shown). It is installed in the cylinder 105 and the upper inner cylinder 106.
  • the single crystal is grown in the lower inner cylinder 105 and the upper inner cylinder 106. Accordingly, the lower inner cylinder 105 and the upper inner cylinder 106 are required to have high corrosion resistance, and thus need to be molded with platinum.
  • the platinum molded product is preferably the lower inner cylinder 105 and the upper inner cylinder 106 of the pressure vessel 119.
  • the size of the lower inner cylinder 105 varies depending on the size of the pressure vessel. For example, it is a medium-sized pressure vessel and has an inner diameter of 20 to 70 mm and a capacity of 0.1 to 8 l. A large pressure vessel with an inner diameter of 70 to 150 mm and a capacity of 8 to 50 l.
  • the surface treatment of the lower inner cylinder 105 can be performed either before installation on the main body 1 of the pressure vessel 119 or after installation on the main body 1 of the pressure vessel 119.
  • the surface on which the coating layer is provided can be either the inner surface or the outer surface of the lower inner cylinder 105, or both.
  • the inner cylinder 105 can be appropriately selected according to various conditions such as dimensions, applications, and reaction conditions. Even if the thickness of the lower inner cylinder 105 is reduced to, for example, 0.2 to 1.0 mm, the attachment and detachment work into the main body 1 is facilitated.
  • the lower inner cylinder 105 can be easily handled, and the attachment and removal work of the pressure vessel 119 in the main body 1 is facilitated.
  • a coating layer on at least the inner surface of the lower inner cylinder 105, it is possible to prevent grain growth and intergranular corrosion in a high-temperature reducing atmosphere, and a reaction with higher purity. A product can be obtained. Furthermore, by nitriding the coating layer, the physical strength can be further improved, and the purity of the reaction product obtained by the low temperature synthesis method can be further increased.
  • the surface on which the coating layer is provided can be the inner surface of the lower inner cylinder 105.
  • the pyrolysis step is preferably pyrolyzed in a flame of a gas burner to form the coating layer as a coating layer.
  • the pressure vessel having the platinum lower inner cylinder 105 already installed at the work site can be cured on the inner surface of the lower inner cylinder 105 without being moved from the work site. It can be set as the pressure vessel corresponding to.
  • the surface of the coating layer is further nitrided by adding nitrogen or hydrogen gas to which this nitrogen or hydrogen is added and heated from the outside, thereby further improving the physical strength, and by using a low-temperature synthesis method. The purity of the reaction product can be further increased.
  • the surface of the platinum molded product is preferably the upper inner cylinder 106 disposed on the lid 2 of the pressure vessel 119.
  • the production of impurities can be further suppressed, and a reaction product with high purity can be obtained.
  • the platinum molded product is preferably a shelf 108 accommodated in the main body 1 of the pressure vessel 119.
  • the material thickness of the shelf 108 can be reduced to, for example, 0.2 to 1.0 mm. Even if the shelf 108 is made thin, it can be prevented from being deformed by its own weight. Further, the shelf 108 can be easily handled, and the operation of storing and taking out the pressure vessel 119 into the main body 1 is facilitated. Further, the shelf 108 can be integrally formed of platinum.
  • the dimensions of the shelf 108 vary depending on the size of the pressure vessel.
  • the shelf 108 is a medium-sized pressure vessel having an inner diameter of 20 to 70 mm and a height of 300 to 2000 mm. A large pressure vessel with an inner diameter of 70 to 150 mm and a height of 2000 to 3000 mm.
  • the surface on which the coating layer 30 is provided is preferably the entire surface of the shelf 108 accommodated in the main body 1 of the pressure vessel 119.
  • a coating layer By forming a coating layer on the entire surface of the constituent parts of the shelf 108, when used in the low temperature synthesis method, grain growth and intergranular corrosion in a high temperature reducing atmosphere can be prevented, and a reaction with higher purity can be achieved. A product can be obtained. Furthermore, by nitriding the coating layer, the purity of the reaction product can be further improved and the physical strength can be increased.
  • FIG. 3 is a cross-sectional view showing an example of a pressure vessel having an inner cylinder vessel.
  • the pressure vessel 19 shown in FIG. 3 has the same basic configuration as the pressure vessel shown in FIG.
  • An inner cylinder container 8 is accommodated in the main body 1 of the pressure container 19 shown in FIG.
  • the inner cylinder container 8 is a sealable cylindrical container made of platinum.
  • a bellows 12 for pressure adjustment is attached to the upper portion of the inner cylinder container 8 in a sealed state.
  • a shelf 108 and a solvent (not shown) illustrated in FIG. 2 are accommodated inside the inner cylinder container 8.
  • the single crystal is grown in the inner cylinder container 8. Therefore, in the pressure vessel 19 shown in FIG.
  • the lower anticorrosion lining 5 and the upper anticorrosion lining 6 do not directly touch the treatment liquid, and therefore do not require high corrosion resistance as required for the inner cylinder.
  • platinum is particularly preferable, the present invention is not limited to this.
  • nickel-based alloys such as the trade names “HASTELLOY” and “INCONEL”, titanium, titanium alloys, tantalum, and tantalum alloys can be used.
  • the size of the inner cylinder container 8 varies depending on the size of the pressure container, but is, for example, a medium-sized pressure container having an inner diameter of 20 to 70 mm and a capacity of 0.1 to 8 l. A large pressure vessel with an inner diameter of 70 to 150 mm and a capacity of 8 to 50 l.
  • the platinum molded product is preferably the inner cylinder container 8 of the pressure vessel 19.
  • the thickness of the inner cylinder container 8 can be reduced to, for example, 0.2 to 1.0 mm. Even if the thickness of the inner cylinder container 8 is reduced, it can be prevented from being deformed by its own weight. Moreover, it becomes easy to handle the inner cylinder container alone, and the operation of storing and taking out the pressure container 19 into the main body 1 is facilitated. Furthermore, since the inner cylinder container 8 and the bellows 12 can be integrally formed of platinum, complicated joining between the inner cylinder container 8 and the bellows 12 becomes unnecessary, and the pressure resistance of the inner cylinder container 8 can be further increased. it can.
  • the surface on which the coating layer 30 is provided can be either one or both of the inner surface and the outer surface of the inner cylinder container 8 of the pressure vessel 19, and depends on various conditions such as the dimensions, applications, reaction conditions, etc. of the inner cylinder container 8 Can be selected as appropriate.
  • a coating layer on at least the inner surface of the inner cylinder container 8
  • grain growth and intergranular corrosion in a high-temperature reducing atmosphere can be prevented, and a reaction with higher purity can be achieved.
  • a product can be obtained.
  • the purity of the reaction product can be further improved and the physical strength can be increased.
  • FIG. 4 is a cross-sectional view showing an example of a large pressure vessel.
  • the pressure vessel 900 shown in FIG. 4 has the same basic configuration as the pressure vessel shown in FIG.
  • a lower anticorrosion lining 5 is further disposed between the main body 1 and the lower inner cylinder 105, and an upper anticorrosion lining 6 is also disposed between the lid 2 and the upper inner cylinder 106.
  • the lower anticorrosion lining 5 and the upper anticorrosion lining 6 are made of a nickel-based alloy having excellent pressure resistance, heat resistance and corrosion resistance, such as trade names of Inconel and Hastelloy.
  • the lower anticorrosion lining 5 and the upper anticorrosion lining 6 have a role of preventing the main body 1 from being corroded when the lower inner cylinder 105 and the upper inner cylinder 106 are damaged and a highly corrosive substance flows out. It can be set as the pressure vessel corresponding to high temperature / high pressure conditions.
  • the pressure vessel 119 of FIG. 2 is a medium-sized pressure vessel, you may provide anticorrosion lining in them.
  • the large pressure vessel 900 shown in FIG. 4 has a structure in which the lower anticorrosion lining 5 and the lower inner cylinder 105 are arranged on the inner surface of the main body 1, the surface treatment of the lower inner cylinder 105 inevitably increases in size.
  • the inner cylinder itself can be made thinner. As a result, the amount of expensive platinum used can be reduced, and a great economic advantage can be obtained.
  • FIG. 5 is a partially enlarged cross-sectional view showing a seal portion of the pressure vessel shown in FIG.
  • the platinum molded product surface hardening method according to the present embodiment is suitable for a form in which the platinum molded product 20 is the lower flange 105 a and the upper flange 106 a provided in the opening of the pressure vessel 900.
  • the lower inner cylinder 105 and the lower flange 105a may be integrally formed of platinum, or the lower flange 105a may be formed as a separate part and the lower inner cylinder 105 and the lower flange 105a may be joined.
  • the present embodiment is not limited to the method of joining the lower inner cylinder 105 and the lower flange 105a.
  • a method of joining for example, as shown in FIG. 5, there is a method in which a flange mounting portion T is provided on the opening periphery of the lower inner cylinder 105 and the lower flange 105 a is attached thereon by welding or diffusion joining.
  • the upper inner cylinder 106 and the upper flange 106a may be integrally formed of platinum, or the upper flange 106a is formed as a separate part, and the upper inner cylinder 106 is formed. And the upper flange 106a may be joined.
  • the surface on which the coating layer is provided is preferably the surface of the portion S that becomes at least a seal portion of the lower flange 105a and the upper flange 106a.
  • the coating layer should just be formed in the surface of the part S used as a seal location at least, More preferably, it is a form which coat
  • the flange as the platinum molded product is connected to the lower flange 105 a attached to the lower inner cylinder 105 shown in FIG. 4. It is not limited, For example, the lower flange 5a and the upper flange 6a which were formed in the lower anticorrosion lining 5 and the upper anticorrosion lining 6 shown in FIG. 3 are included.
  • the coating solution used in the first coating step is blended with an iridium salt or ruthenium salt and a platinum compound such as chloroplatinic acid to form a coating layer made of an alloy of iridium or ruthenium and platinum. It is preferable to do.
  • the adhesion between the platinum molded product and the coating layer is increased, and the physical strength can be further improved.
  • the surface hardness and physical strength can be raised more by carrying out the nitriding process of the surface of the coating layer 30.
  • the surface of the platinum molded product whose surface is hardened according to the present embodiment is the upper flange 106a and the lower flange 105a in FIG. 4, the upper flange 6a and the lower flange 5a in FIG. 3, JIS Z 2244: 2009
  • the surface Vickers hardness measured according to the above is preferably 300 Hv to 500 Hv. More preferably, it is 350 Hv to 450 Hv. If it is less than 300 Hv, a large deformation (collapse) may occur due to tightening, and sufficient sealing may not be achieved. In addition, the surface hardness may be lower than that of the gasket, and the flange may be deformed to shorten the life of the pressure vessel. If it exceeds 500 Hv, cracks may occur. Furthermore, it may break.
  • the platinum molded product is preferably a crucible.
  • the platinum crucible is used for the purpose of preventing contamination of trace impurities such as single crystal growth of various oxides and melting of optical glass.
  • the platinum molded product 20 includes a so-called reinforced platinum crucible in which an oxide such as zirconia (ZrO 2 ) is dispersed.
  • the surface on which the coating layer 30 is provided can be either one or both of the inner surface and the outer surface of the crucible, and can be appropriately selected according to various conditions such as the size of the crucible, application, and reaction conditions.
  • the thickness of the crucible can be reduced to 0.2 to 1.0 mm, for example.
  • the crucible Even if the thickness of the crucible is reduced, the crucible can be prevented from being deformed by its own weight. In addition, the crucible can be handled easily. Furthermore, durability in a reducing atmosphere is improved. Furthermore, by nitriding the coating layer 30, the purity of the reaction product can be further improved, and the physical strength can be increased.
  • the dimensions of the crucible are, for example, an inner diameter of 25 to 100 mm, a height of 25 to 150 mm, and a capacity of 0.01 to 2 l. In addition, this embodiment is not restrict
  • Example 1 As a platinum molded product, an inner cylinder of a bottomed cylindrical pressure vessel having one end opened with platinum having a diameter (inner dimension) of 30 mm, a height of 200 mm, and a thickness of 0.2 mm was formed. Iridium chloride and chloroplatinic acid were mixed at a molar ratio of 80:20, dissolved in butanol, and a solution having a total molar concentration of iridium and platinum of 0.25 mol-Ir + Pt / l was used as a coating solution. The obtained coating solution was applied to the inner surface of the inner cylinder, allowed to stand at 60 ° C. for 10 minutes, and dried to form a coating layer.
  • the coating amount per one time was 20 ml / m 2 .
  • an iridium-platinum alloy film having a thickness of 0.1 ⁇ m was obtained.
  • heating was performed so that the maximum temperature of the heat-treated surface at the center of the portion exposed to the flame was in the range of 600 to 750 ° C., and the treatment time was 10 minutes.
  • the flame temperature was measured using a radiation thermometer (model AD-5616, manufactured by A & D).
  • the coating from coating to thermal decomposition was repeated 10 times to form a coating layer made of iridium-platinum alloy having a thickness of 1.0 ⁇ m.
  • the surface of the coating layer was further heated by using a gas burner flame in an air atmosphere to carry out a stabilization treatment.
  • heating was performed so that the maximum temperature of the heat-treated surface at the center of the portion exposed to the flame was in the range of 750 to 900 ° C., and the treatment time was 20 minutes.
  • the obtained inner cylinder has increased surface hardness and is easy to attach to the pressure vessel body. Further, since the inner surface was coated with an iridium-platinum alloy, it was possible to form an inner cylinder that hardly caused grain growth and intergranular corrosion even when used as a container for the low temperature synthesis method.
  • Example 2 As a platinum molded product, a flange having a diameter of 70 mm and a thickness of 2.0 mm was formed on the outer peripheral edge of the opening of the platinum inner cylinder. Ruthenium chloride and chloroplatinic acid were mixed at a molar ratio of 1: 1, dissolved in butanol, and a solution having a total molar concentration of ruthenium and platinum of 0.5 mol-Ru + Pt / l was used as the first coating solution. . The obtained first coating solution was applied to the surface of the flange facing the flange (upper flange) on the lid side, allowed to stand at 40 ° C. for 15 minutes, and dried to form a coating layer.
  • the coating amount per one time was 20 ml / m 2 .
  • a 0.2 ⁇ m thick ruthenium-platinum alloy film was obtained.
  • heating was performed so that the maximum temperature of the heat-treated surface at the center of the portion exposed to the flame was in the range of 550 to 650 ° C., and the treatment time was 30 minutes. From application of the first coating solution to thermal decomposition was repeated 5 times to form a first coating layer made of ruthenium-platinum having a thickness of 1.0 ⁇ m.
  • ruthenium chloride and rhodium chloride are blended at a molar ratio of 1: 1, dissolved in butanol, and a solution having a total molar concentration of ruthenium and rhodium of 1.0 mol-Ru + Rh / l is used as the second coating solution.
  • the obtained 2nd coating liquid was apply
  • the coating amount per one time was 0.5 ⁇ m.
  • the surface of the coating layer was heat-treated using a gas burner flame in the air atmosphere and thermally decomposed to obtain a ruthenium-rhodium alloy film having a thickness of 0.5 ⁇ m.
  • the second pyrolysis step heating was performed so that the maximum temperature of the heat-treated surface at the center of the portion exposed to the flame was in the range of 650 to 750 ° C., and the treatment time was 30 minutes.
  • the application from the second coating solution to thermal decomposition was repeated 20 times to form a second coating layer made of ruthenium-rhodium having a thickness of 10 ⁇ m.
  • the stabilization process was performed using an electric furnace with a muffle in an air atmosphere at an atmospheric temperature of 700 ° C. and a processing time of 2 hours.
  • the obtained flange having a hardened surface apparently had a slightly different color tone from platinum, and showed a slightly blackish metallic luster.
  • the Vickers hardness was measured according to JIS Z 2244: 2009, it was 350 to 380 Hv, and it was confirmed that the surface hardness was sufficient as a flange.
  • Example 3 As a platinum molded product, a crucible having a diameter (inner dimension) of 70 mm, a height of 100 mm, and a thickness of 0.8 mm was molded. Iridium chloride was dissolved in butanol, and a solution having a molar concentration of iridium of 0.5 mol-Ir / l was used as a coating solution. The obtained coating solution was applied to the inner and outer surfaces of the crucible, allowed to stand at 40 to 50 ° C. for 10 minutes, and dried to form a coating layer. The coating amount per one time was 20 ml / m 2 .
  • a iridium metal film having a thickness of 0.1 ⁇ m was obtained.
  • heating was performed so that the maximum temperature of the heat-treated surface at the center of the portion exposed to the flame was in the range of 800 to 850 ° C., and the treatment time was 20 minutes.
  • the coating liquid coating to thermal decomposition was repeated 10 times to form a coating layer made of iridium metal and having a thickness of 1.0 ⁇ m.
  • the surface of the coating layer was further heated in an air atmosphere using a flame of a gas burner to perform a stabilization treatment.
  • the maximum temperature of the heat-treated surface at the center of the portion exposed to the flame was in the range of 850 to 900 ° C., and the treatment time was 40 minutes.
  • the resulting crucible had increased surface hardness and improved handling.
  • Example 4 In Example 1, iridium chloride and ruthenium chloride were blended in a molar ratio of 80:20, dissolved in butanol, and a solution having a total molar concentration of iridium and ruthenium of 0.5 mol-Ir + Ru / l was applied as a coating solution. Except that, the surface of the inner cylinder of the pressure vessel, which is a platinum molded product, was cured according to Example 1. The inner surface of the obtained inner cylinder was coated with an iridium-ruthenium alloy. The obtained inner cylinder has increased surface hardness and is easy to attach to the pressure vessel body.
  • the Vickers hardness was measured according to JIS Z 2244: 2009 in the same manner as in Example 2, and it was 380 to 400 Hv.
  • Example 5 In Example 2, after the stabilization treatment, the entire surface of the flange surface was nitrided by holding in pure nitrogen gas at 1100 ° C. for 3 hours. The thickness of the nitriding layer was about 5 ⁇ m. When the Vickers hardness of the surface of the nitrided layer was measured according to JIS Z 2244: 2009, it was 420 to 450 Hv, and it was confirmed that the surface hardness was improved as compared with the flange obtained in Example 2.
  • the surface hardening method for a platinum molded product according to the present invention can ensure physical strength even if the platinum molded product is thin, for example, 0.2 to 1.0 mm.
  • the inner surface of the platinum molded article an alloy containing at least one of iridium, ruthenium or iridium or ruthenium, platinum grain growth and intergranular corrosion can be prevented even in a reducing atmosphere such as a thermal synthesis method. It can be prevented and a chemically stable platinum molded article can be obtained.
  • the surface-curing method for a platinum molded product according to the present invention is suitable for curing the inner surface, outer surface, or inner / outer surface of an inner cylinder, a flange, and a crucible of a pressure vessel, for example.
  • the surface hardening method of the platinum molded product according to the present invention is suitable for curing the surface of a platinum molded product such as platinum tongs and evaporating dishes.

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Abstract

La présente invention concerne un article moulé en platine qui présente une surface durcie et une excellente résistance à la déformation par son poids propre, même si l'article moulé en platine est mince, il se déforme peu et il est facile à manipuler, il présente une résistance à la corrosion et une bonne durabilité sous des températures et pressions élevées et peut empêcher la croissance de particules de platine et la corrosion des limites des particules dans une atmosphère réductrice. L'invention concerne également un procédé permettant de durcir la surface d'un article moulé en platine. Le procédé de durcissement de la surface d'un article moulé en platine comprend : une étape d'application permettant de former une couche d'application par l'application d'une solution d'application qui contient un sel d'iridium et/ou un sel de ruthénium à la surface d'un article moulé en platine (20) ; et une étape de pyrolyse destinée à la pyrolyse de la couche d'application dans une atmosphère de gaz d'azote ou dans une flamme afin de convertir la couche d'application en une couche de revêtement (30) qui comprend de l'iridium, du ruthénium ou un alliage contenant de l'iridium et/ou du ruthénium.
PCT/JP2011/063924 2010-06-29 2011-06-17 Procédé de durcissement de surface d'article moulé en platine et article moulé en platine présentant une surface durcie Ceased WO2012002176A1 (fr)

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Citations (6)

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JPH1123374A (ja) * 1997-06-27 1999-01-29 Tokyo Electron Ltd 熱処理炉用温度計
JP2002060296A (ja) * 2000-08-21 2002-02-26 Crystal System:Kk 単結晶製造用るつぼおよび単結晶製造装置ならびにこれを用いた単結晶の製造方法
JP2005154805A (ja) * 2003-11-21 2005-06-16 Furuya Kinzoku:Kk 耐食材
JP2005154818A (ja) * 2003-11-25 2005-06-16 Furuya Kinzoku:Kk 耐食材及びその製造方法
JP2006002248A (ja) * 2004-05-18 2006-01-05 Kuwayama Corp 硬化白金装飾品
JP2008162819A (ja) * 2006-12-27 2008-07-17 Mitsubishi Chemicals Corp ハロゲン化ガリウムペンタアンモニエートとその製造方法、および窒化ガリウム単結晶の製造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1123374A (ja) * 1997-06-27 1999-01-29 Tokyo Electron Ltd 熱処理炉用温度計
JP2002060296A (ja) * 2000-08-21 2002-02-26 Crystal System:Kk 単結晶製造用るつぼおよび単結晶製造装置ならびにこれを用いた単結晶の製造方法
JP2005154805A (ja) * 2003-11-21 2005-06-16 Furuya Kinzoku:Kk 耐食材
JP2005154818A (ja) * 2003-11-25 2005-06-16 Furuya Kinzoku:Kk 耐食材及びその製造方法
JP2006002248A (ja) * 2004-05-18 2006-01-05 Kuwayama Corp 硬化白金装飾品
JP2008162819A (ja) * 2006-12-27 2008-07-17 Mitsubishi Chemicals Corp ハロゲン化ガリウムペンタアンモニエートとその製造方法、および窒化ガリウム単結晶の製造方法

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