# US 10,766,824 B2 · Methods of minimizing particles on wafer from plasma spray coatings > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,766,824 B2 - Document ID: US10766824B2 - Status: Granted - Kind: B2 - Application number: 15/807,508 - Filed: 2017-11-08 - Published: 2019-05-09 - Granted: 2020-09-08 - Earliest claimed: 2017-11-08 - Assignees: Applied Materials, Inc. - Applicants: APPLIED Materials, Inc. - Inventors: Kaushal Gangakhedkar; Jennifer Y. Sun; Xiao-Ming He - Web page: https://patentgrep.com/patent/US10766824B2 ## CPC - C04B 35/64: Burning or sintering processes (C04B33/32 takes precedence {; powder metallurgy B22F}) - C04B 35/50: based on rare-earth compounds {(non-oxide rare earth compounds C04B35/5156)} - C04B 35/505: based on yttrium oxide - C04B 35/62222: {obtaining ceramic coatings (coating of mortars, concrete, artificial or natural stone or ceramics C04B41/45; laminated ceramic products B32B18/00; coating of glass C03C17/00, applying ceramic coatings on silicon for semi-conductor purposes H10W; coating metallic materials C23)} - C04B 41/009: {characterised by the material treated} - C04B 41/5031: {Alumina} - C04B 41/5032: {Aluminates (aluminate spinels C04B41/5046)} - C04B 41/5042: {Zirconium oxides or zirconates; Hafnium oxides or hafnates} - C04B 41/5045: {Rare-earth oxides} - C04B 41/5055: {Fluorides} - C04B 41/87: Ceramics - H01J 37/32467: {Material} - H01J 37/32495: {Means for protecting the vessel against plasma} - C04B 2235/3217: Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina - C04B 2235/3222: Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4) - C04B 2235/3224: Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide - C04B 2235/3225: Yttrium oxide or oxide-forming salts thereof - C04B 2235/3244: Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof - C04B 2235/3246: Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia - C04B 2235/3418: Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint - C04B 2235/445: Fluoride containing anions, e.g. fluosilicate - C04B 2235/6562: Heating rate - C04B 2235/6565: Cooling rate - C04B 2235/6567: Treatment time - C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE - H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H) ## Abstract Methods comprise performing two or more thermal cycles on an article comprising a body and a ceramic coating. Each thermal cycle of the two or more thermal cycles comprise heating the ceramic article to a target temperature at a first ramping rate. Each thermal cycle further comprises maintaining the article at the target temperature for a first duration of time and then cooling the article to a second target temperature at a second ramping rate. The method further comprises submerging the article in a bath for a second duration of time to remove the particles from the ceramic coating. ## Claims ### Claim 1 A method comprising: performing two or more successive thermal cycles on a ceramic article comprising a body and a ceramic coating on at least one surface of the body, wherein the two or more successive thermal cycles expand and contract the ceramic coating to weaken bonds of particles to the ceramic coating, and wherein each successive thermal cycle of the two or more successive thermal cycles comprises: heating the ceramic article to a first target temperature of about 100° C. to about 150° C. at a first ramping rate; maintaining the ceramic article at the first target temperature for a first duration of time; and cooling the ceramic article to a second target temperature at a second ramping rate; and responsive to performing the two or more successive thermal cycles, submerging the ceramic article in a bath for a second duration of time to remove the particles from the ceramic coating. ### Claim 2 (depends on 1) The method of claim 1, wherein the ceramic coating consists essentially of at least one of Y2O3, Al2O3, Er2O3, Gd2O3, YF3, Nd2O3, Er4Al2O9, Er3A15O12, ErAlO3, Gd4A12O9, GdAlO3, Nd3A15O12, Nd4A12O9, NdAlO3, YAlO3, Y4Al2O9, Y3A15O12 (YAG), a solid solution of Y2O3—ZrO2, a ceramic compound comprising Y4Al2O9 and a solid-solution of Y2O3—ZrO2, or a ceramic compound comprising Y2O3, Er2O3, ZrO2, Gd2O3 and SiO2. ### Claim 3 (depends on 1) The method of claim 1, wherein the first ramping rate is about 3° C. per minute to about 10° C. per minute. ### Claim 4 (depends on 1) The method of claim 1, wherein the second target temperature is about 24° C. to 27° C. ### Claim 5 (depends on 1) The method of claim 1, wherein the second ramping rate is about 2° C. per minute to about 10° C. per minute. ### Claim 6 (depends on 1) The method of claim 1, wherein the bath is a bath of deionized water, and wherein submerging the ceramic article in the bath of deionized water for the second duration of time comprises ultrasonicating the ceramic article at a frequency of about 40 kHz to about 60 kHz for the second duration of time. ### Claim 7 (depends on 1) The method of claim 1, wherein the ceramic article is a chamber component for a processing chamber. ### Claim 8 A method comprising: performing two or more thermal cycles on a ceramic article comprising a body and a ceramic coating on at least one surface of the body, wherein the two or more thermal cycles expand and contract the ceramic coating to weaken bonds of particles to the ceramic coating, and wherein each thermal cycle of the two or more thermal cycles comprises: heating the ceramic article to a target temperature of about 100° C. to about 150° C. at a first ramping rate of about 3° C. per minute to about 10° C. per minute; maintaining the ceramic article at the target temperature for a first duration of time of about 5 minutes to about 20 minutes; cooling the ceramic article to a second target temperature of about 24° C. to 27° C. at a second ramping rate of about 2° C. per minute to about 10° C. per minute; and maintaining the ceramic article at the second target temperature for a second duration of time of about 2 seconds to about 20 minutes; and submerging the ceramic article in a bath for a third duration of time to remove the particles from the ceramic coating. ### Claim 9 A method comprising: performing two or more thermal cycles on a ceramic article comprising a body and a ceramic coating on at least one surface of the body, wherein the two or more thermal cycles expand and contract the ceramic coating to weaken bonds of particles to the ceramic coating, and wherein each thermal cycle of the two or more thermal cycles comprises: heating the ceramic article to a first target temperature of about 100° C. to about 150° C. at a first ramping rate; maintaining the ceramic article at the first target temperature for a first duration of time, wherein the first duration of time is about 5 minutes to about 20 minutes; and cooling the ceramic article to a second target temperature at a second ramping rate; and submerging the ceramic article in a bath for a second duration of time to remove the particles from the ceramic coating. ### Claim 10 (depends on 9) The method of claim 9, wherein the ceramic coating consists essentially of at least one of Y2O3, Al2O3, Er2O3, Gd2O3, YF3, Nd2O3, Er4A12O9, Er3A15O12, ErAlO3, Gd4A12O9, GdAlO3, Nd3A15O12, Nd4A12O9, NdAlO3, YAlO3, Y4Al2O9, Y3A15O12 (YAG), a solid solution of Y2O3—ZrO2, a ceramic compound comprising Y4Al2O9 and a solid-solution of Y2O3—ZrO2, or a ceramic compound comprising Y2O3, Er2O3, ZrO2, Gd2O3 and SiO2. ### Claim 11 (depends on 9) The method of claim 9, wherein the first ramping rate is about 3° C. per minute to about 10° C. per minute. ### Claim 12 (depends on 9) The method of claim 9, wherein the second ramping rate is about 2° C. per minute to about 10° C. per minute. ### Claim 13 (depends on 1, 9) The method of claim 9, The method of claim 1, wherein the second target temperature is about 24° C. to about 27° C. ### Claim 14 (depends on 9) The method of claim 9, wherein the bath is a bath of deionized water, and wherein submerging the ceramic article in the bath of deionized water for the second duration of time comprises ultrasonicating the ceramic article at a frequency of about 40 kHz to about 60 kHz for the second duration of time. ### Claim 15 (depends on 9) The method of claim 9, wherein the ceramic article is a chamber component for a processing chamber. ### Claim 16 (depends on 9) The method of claim 9, wherein the two or more thermal cycles are consecutive thermal cycles. ### Claim 17 A method comprising: performing two or more thermal cycles on a ceramic article comprising a body and a ceramic coating on at least one surface of the body, wherein the two or more thermal cycles expand and contract the ceramic coating to weaken bonds of particles to the ceramic coating, and wherein each thermal cycle of the two or more thermal cycles comprises: heating the ceramic article to a first target temperature of about 100° C. to about 150° C. at a first ramping rate; maintaining the ceramic article at the first target temperature for a first duration of time; and cooling the ceramic article to a second target temperature at a second ramping rate; and submerging the ceramic article in a bath for a second duration of time to remove the particles from the ceramic coating, wherein the bath is a bath of deionized water, and wherein submerging the ceramic article in the bath of deionized water for the second duration of time comprises alternating between ultrasonicating the ceramic article at a first frequency of about 40 kHz to about 60 kHz for a third duration of time and ultrasonicating the ceramic article at a second frequency of about 100 kHz to about 140 kHz for a fourth duration of time. ### Claim 18 (depends on 17) The method of claim 17, wherein the first ramping rate is about 3° C. per minute to about 10° C. per minute and the second ramping rate is about 2° C. per minute to about 10° C. per minute. ### Claim 19 (depends on 17) The method of claim 17, wherein the second target temperature is about 24° C. to about 27° C. ### Claim 20 (depends on 17) The method of claim 17, wherein the ceramic coating consists essentially of at least one of Y2O3, Al2O3, Er2O3, Gd2O3, YF3, Nd2O3, Er4A12O9, Er3A15O12, ErAlO3, Gd4A12O9, GdAlO3, Nd3A15O12, Nd4A12O9, NdAlO3, YAlO3, Y4A12O9, Y3A15O12 (YAG), a solid solution of Y2O3—ZrO2, a ceramic compound comprising Y4A12O9 and a solid-solution of Y2O3—ZrO2, or a ceramic compound comprising Y2O3, Er2O3, ZrO2, Gd2O3 and SiO2.