# US 10,767,251 B2 · Spray material, sprayed member and making method > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,767,251 B2 - Document ID: US10767251B2 - Status: Granted - Kind: B2 - Application number: 16/406,410 - Filed: 2019-05-08 - Published: 2019-11-21 - Granted: 2020-09-08 - Earliest claimed: 2018-05-18 - Assignees: Shin-Etsu Chemical Co., Ltd. - Applicants: Shin-Etsu Chemical Co., Ltd. - Inventors: Yasushi Takai - Web page: https://patentgrep.com/patent/US10767251B2 ## CPC - C23C 4/11: Oxides - C23C 4/06: Metallic material - C23C 4/134: Plasma spraying - C23C 28/042: {including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides} - 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 (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) ## Abstract A spray material is defined as composite particles consisting essentially of (A) particles of rare earth fluoride and (B) particles of rare earth oxide, hydroxide or carbonate, consolidated together. The spray material is plasma sprayed onto a substrate to form a sprayed layer containing rare earth oxyfluoride in a consistent manner while minimizing the process shift and releasing few particles. The sprayed member has improved corrosion resistance to halogen-based gas plasma. ## Claims ### Claim 1 A spray material comprising composite particles comprising (A) particles of rare earth fluoride and (B) particles of at least one rare earth compound selected from rare earth oxide, rare earth hydroxide, and rare earth carbonate, wherein the particles (A) and the particles (B) are consolidated together, wherein a crystal phase of the spray material comprises a first phase corresponding to the rare earth fluoride and a second phase corresponding to the at least one rare earth compound, and wherein the crystal phase of the spray material does not contain a phase corresponding to rare earth oxyfluoride. ### Claim 2 (depends on 1) The spray material of claim 1 wherein the composite particles comprise 5% to 40% by weight of the particles (B) with the balance being the particles (A), based on the total weight of the particles (A) and the particles (B). ### Claim 3 (depends on 1) The spray material of claim 1 further comprising 0.05% to 3% by weight of an organic binder selected from rare earth organic compounds and organic polymers, based on the total weight of the particles (A) and the particles (B). ### Claim 4 (depends on 1) The spray material of claim 1, having a water content of up to 2% by weight. ### Claim 5 (depends on 1) The spray material of claim 1, having an average particle size of 10 μm to 60 μm. ### Claim 6 (depends on 1) The spray material of claim 1, having a specific surface area of 1.5 m2/g to 5 m2/g. ### Claim 7 (depends on 1) The spray material of claim 1, having a bulk density of 0.8 g/cm3 to 1.4 g/cm3. ### Claim 8 (depends on 1) The spray material of claim 1, wherein a rare earth element in each of the rare earth fluoride, the rare earth oxide, the rare earth hydroxide, and the rare earth carbonate is at least one element selected from Y and Group 3 elements from La to Lu. ### Claim 9 (depends on 1) A sprayed member comprising a substrate and a sprayed coating disposed thereon, the sprayed coating including a sprayed layer formed by plasma spraying of the spray material of claim 1. ### Claim 10 (depends on 1) A sprayed member comprising a substrate and a sprayed coating disposed thereon, the sprayed coating including an undercoat and a sprayed layer formed by atmospheric plasma spraying of the spray material of claim 1, the sprayed layer constituting at least an outermost layer. ### Claim 11 (depends on 10) The sprayed member of claim 10 wherein the undercoat is composed of a single layer or a plurality of layers, each layer being selected from a rare earth fluoride layer and a rare earth oxide layer. ### Claim 12 (depends on 9) The sprayed member of claim 9 wherein the sprayed layer has a thickness of 150 μm to 350 μm. ### Claim 13 (depends on 9) The sprayed member of claim 9 wherein the sprayed layer contains a rare earth oxyfluoride phase as a main phase and a phase of a rare earth compound other than the rare earth oxyfluoride as an auxiliary phase. ### Claim 14 (depends on 13) The sprayed member of claim 13 wherein the rare earth oxyfluoride as the main phase is Re5O4F7, and wherein Re is a rare earth element inclusive of Y. ### Claim 15 (depends on 13) The sprayed member of claim 13 wherein the rare earth compound other than the rare earth oxyfluoride contains both rare earth oxide and rare earth fluoride. ### Claim 16 (depends on 9) The sprayed member of claim 9 wherein the sprayed layer has a volume resistivity at 200° C. and a volume resistivity at 23° C., a ratio of the volume resistivity at 23° C. to the volume resistivity at 200° C. ranging from 0.1 to 30. ### Claim 17 (depends on 9) The sprayed member of claim 9 wherein a rare earth element in each of the rare earth fluoride, the rare earth oxide, the rare earth hydroxide, and the rare earth carbonate is at least one element selected from Y and Group 3 elements from La to Lu. ### Claim 18 (depends on 1) A method for preparing a sprayed member, comprising the step of forming a sprayed layer on a substrate by atmospheric plasma spraying of the spray material of claim 1. ### Claim 19 (depends on 1) The spray material of claim 1, wherein the spray material is prepared by mixing the particles (A) and the particles (B) without a heat treatment where the particles (A) and the particles (B) are exposed to a temperature of 180° C. or higher. ### Claim 20 (depends on 1) The spray material of claim 1, having a specific surface area of 2.1 m2/g to 5 m2/g.