# US 11,078,567 B2 · Process for manufacturing a part made of nickle-based superalloy containing hafnium > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,078,567 B2 - Document ID: US11078567B2 - Status: Granted - Kind: B2 - Application number: 16/308,245 - Filed: 2017-06-09 - Published: 2019-05-23 - Granted: 2021-08-03 - Earliest claimed: 2016-06-10 - Assignees: Safran - Applicants: Safran - Inventors: Amar Saboundji; Virginie Jaquet - Web page: https://patentgrep.com/patent/US11078567B2 ## CPC - C23C 14/5846: {Reactive treatment} - C22C 19/057: {with the maximum Cr content being less 10%} - C23C 10/28: using solids, e.g. powders, pastes - C23C 14/165: {by cathodic sputtering} - 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) - C22C: ALLOYS (treatment of alloys C21D, C22F) ## Abstract The invention relates to a process for manufacturing a part made of nickel-based monocrystalline superalloy containing hafnium. This process is noteworthy in that it comprises the following successive steps consisting in: —manufacturing a nickel-based monocrystalline superalloy that is not doped with hafnium, —manufacturing a part from this superalloy, —directly depositing on said part a layer of hafnium having a thickness of between 50 nm and 800 nm, —carrying out a diffusion treatment of the hafnium so as to form an interdiffusion layer at the surface of said part and to thus obtain a part made of nickel-based monocrystalline superalloy containing hafnium. ## Claims ### Claim 1 A process for manufacturing a hafnium-containing nickel-based single-crystal superalloy part, wherein the process comprises the following successive steps: manufacturing a nickel-based, non-hafnium-doped, single-crystal superalloy, manufacturing a part from this superalloy, depositing, directly on said part, a layer of nanocrystalline or microcrystalline hafnium having a thickness comprised between 50 nm and 800 nm, carrying out a hafnium diffusion treatment so as to form an interdiffusion layer on the surface of said part, and thereby obtain a hafnium-containing nickel-based single-crystal superalloy part. ### Claim 2 (depends on 1) The process according to claim 1, wherein the deposition of the layer of hafnium is carried out by physical vapour deposition (PVD). ### Claim 3 (depends on 2) The process according to claim 2, wherein the deposition of the layer of hafnium is carried out by cathode sputtering. ### Claim 4 (depends on 1) The process according to claim 1, wherein the deposition of the layer of hafnium is carried out by chemical vapour deposition (CVD). ### Claim 5 (depends on 1) The process according to claim 1, wherein the layer of hafnium deposited on said part has a thickness comprised between 50 nm and 300 nm. ### Claim 6 (depends on 1) The process according to claim 1, wherein the hafnium diffusion treatment is carried out under vacuum or under a mixture of 95% by volume argon and 5% by volume helium, by carrying out a temperature increase until bringing said part to a temperature comprised between 500° C. and 1,200° C., maintaining this temperature for 1 hour to 4 hours and cooling said part until it returns to room temperature. ### Claim 7 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises in mass percent 5.2% aluminium, 6.5% cobalt, 7.8% chromium, 2% molybdenum, 7.9% tantalum, 1.1% titanium, 5.7% tungsten and the remainder nickel. ### Claim 8 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises in mass percent 5.6% aluminium, 9.6% cobalt, 6.5% chromium, 0.6% molybdenum, 3% rhenium, 6.5% tantalum, 1% titanium, 6% tungsten and the remainder nickel. ### Claim 9 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises in mass percent 5.73% aluminium, 9.6% cobalt, 3.46% chromium, 0.6% molybdenum, 4.9% rhenium, 8.3% tantalum, 0.9% titanium, 5.5% tungsten and the remainder nickel. ### Claim 10 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises in mass percent 5.7% aluminium, 3% cobalt, 2% chromium, 0.4% molybdenum, 6% rhenium, 8% tantalum, 0.2% titanium, 5% tungsten, 0.1% niobium and the remainder nickel. ### Claim 11 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped single-crystal nickel-based superalloy comprises in mass percent 5.8% aluminium, 12.5% cobalt, 4.2% chromium, 1.4% molybdenum, 5.4% rhenium, 7.2% tantalum, 6% tungsten and the remainder nickel. ### Claim 12 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises in mass percent 6% aluminium, less than 0.2% cobalt, 4% chromium, 1% molybdenum, 4% rhenium, 5% tantalum, 0.5% titanium, 5% tungsten, 4% ruthenium and the remainder nickel. ### Claim 13 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises nickel, aluminium, cobalt, chromium, molybdenum, tantalum and tungsten. ### Claim 14 (depends on 1) The process according to claim 1, wherein the non-hafnium-doped nickel-based single-crystal superalloy comprises in mass percent about 5.2% to 6% aluminium, about 0.2% to 12.5% cobalt, about 2% to 7.8% chromium, about 0.4% to 2% molybdenum, about 5% to 8% tantalum and about 5% to 6% tungsten. ### Claim 15 (depends on 1) The process according to claim 1, wherein the part is manufactured from the non-hafnium-doped nickel-based single-crystal superalloy by casting or additive manufacturing. ### Claim 16 (depends on 1) The process according to claim 1, wherein the deposited layer of hafnium is a layer containing at least 99.99 atomic percent of hafnium. ### Claim 17 (depends on 1) The process according to claim 1, wherein after the manufacturing step of the part from the non-hafnium-doped nickel-based single-crystal superalloy and before the depositing step of the layer of hafnium, the manufactured part is subjected to a solutioning treatment. ### Claim 18 (depends on 17) The process according to claim 17, wherein the solutioning treatment consists of a first step of temperature increase until reaching a temperature of about 1,100° C. for a period comprised between a few minutes and 4 hours, followed by a second step of temperature increase until reaching a temperature of about 1,200° C. for a period comprised between a few minutes and 4 hours, and finally a third step of temperature increase until reaching a temperature of about 1,300° C. for a period comprised between a few minutes and 4 hours. ### Claim 19 (depends on 1) The process according to claim 1, wherein the deposition of the layer of hafnium is carried out by a technique selected from low-pressure chemical vapour deposition (LPCVD), chemical vapour aluminizing (CVA), ultra-high vacuum chemical vapour deposition (UHVCVD), plasma enhanced chemical vapour deposition (PECVD), atmospheric pressure chemical vapour deposition (APCVD), and atomic layer chemical vapour deposition (ALCVD).