# US 8,465,596 B2 · Supercritical processing apparatus and supercritical processing method > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,465,596 B2 - Document ID: US8465596B2 - Status: Granted - Kind: B2 - Application number: 13/039,361 - Filed: 2011-03-03 - Published: 2011-09-08 - Granted: 2013-06-18 - Earliest claimed: 2010-03-05 - Assignees: Tokyo Electron Limited - Applicants: Takayuki Toshima; Mitsuaki Iwashita; Kazuyuki Mitsuoka; Hidekazu Okamoto; Hideo Namatsu - Inventors: Takayuki Toshima; Mitsuaki Iwashita; Kazuyuki Mitsuoka; Hidekazu Okamoto; Hideo Namatsu - Web page: https://patentgrep.com/patent/US8465596B2 ## CPC - B08B 5/00: Cleaning by methods involving the use of air flow or gas flow (cleaning hollow articles by methods or apparatus specially adapted thereto B08B9/00) - B08B 7/0021: {by liquid gases or supercritical fluids} - B08B 13/00: Accessories or details of general applicability for machines or apparatus for cleaning - H10P 70/20: {Cleaning during device manufacture} - H10P 70/80: {Cleaning only by supercritical fluids} - H10P 72/0402: {Apparatus for fluid treatment (H10P72/0441, H10P72/0448 take precedence)} - H10P 72/0406: {for cleaning followed by drying, rinsing, stripping, blasting or the like} - H10P 72/0408: {for drying} - H10P 72/0414: {using mainly spraying means, e.g. nozzles} - H10P 72/0462: {characterised by the construction of the processing chambers, e.g. modular processing chambers} - B08B: CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL - H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10 ## Abstract Disclosed is a supercritical processing apparatus and a supercritical processing method for suppressing the pattern collapse or the injection of material constituting a processing liquid into a substrate. A processing chamber receives a substrate subjected to a processing with supercritical fluid, and a liquid supply unit supplies a processing liquid including a fluorine compound to the processing chamber. A liquid discharge unit discharges the supercritical fluid from the processing chamber, a pyrolysis ingredient removing unit removes an ingredient facilitating the pyrolysis of a liquid from the processing chamber or from the liquid supplied from the liquid supply unit, and a to heating unit heats the processing liquid including a fluorine compound of hydrofluoro ether or hydrofluoro carbon. ## Claims ### Claim 1 A supercritical processing method, comprising the steps of: loading a substrate formed with a pattern into a processing chamber where the substrate is processed by a processing liquid and by a supercritical liquid including a fluorine compound; removing an ingredient facilitating a pyrolysis of the fluorine compound of the supercritical liquid both from the processing chamber and from the supercritical liquid; supplying the supercritical liquid including the fluorine compound from which the ingredient facilitating the pyrolysis of the fluorine is removed to the processing chamber where the substrate is received; sealing the processing chamber and performing a supercritical processing for the substrate with a supercritical condition obtained by heating the supercritical liquid including the fluorine compound from which the ingredient facilitating the pyrolysis of the fluorine is removed; and discharging the supercritical liquid from the processing chamber after completing the supercritical processing, wherein the removing of the ingredient from the processing chamber is performed in a closed state of the processing chamber prior to the loading of the substrate into the processing chamber and the removing of the ingredient from the supercritical liquid is performed prior to the supplying of the supercritical liquid to the processing chamber, and wherein the fluorine compound is hydrofluoro ether or hydrofluoro carbon. ### Claim 2 (depends on 1) The supercritical processing method as claimed in claim 1, wherein the removing step further comprises supplying inert gas to a storage unit provided independently from the processing chamber to store the supercritical liquid and to perform a bubbling process in the storage unit before supplying the supercritical liquid to the processing chamber. ### Claim 3 (depends on 1) The supercritical processing method as claimed in claim 1, wherein the removing step further comprises supplying inert gas to the processing chamber. ### Claim 4 (depends on 1) The supercritical processing method as claimed in claim 1, wherein the fluorine compound is hydrofluoro ether consisting of a fluoroalkyl group including one or fewer carbon-carbon bond of a carbon atom positioned at α location, and two or fewer carbon-carbon bonds of a carbon atom positioned at β location, when viewed from an oxygen atom. ### Claim 5 (depends on 3) The supercritical processing method as claimed in claim 3, further comprising supplying the inert gas to the processing chamber before the processing chamber is sealed after the substrate is loaded into the processing chamber, in order to remove the ingredient facilitating the pyrolysis of the fluorine compound of the supercritical liquid from the processing chamber. ### Claim 6 (depends on 3) The supercritical processing method as claimed in claim 3, further comprising supplying the inert gas to the processing chamber after the substrate is loaded into the processing chamber, in order to remove the ingredient facilitating the pyrolysis of the fluorine compound of the supercritical liquid from the processing chamber. ### Claim 7 (depends on 3) The supercritical processing method as claimed in claim 3, wherein the processing chamber is received within a case in which the substrate is loaded and unloaded through a loading/unloading port, and further comprises supplying the inert gas to the case while the processing chamber is in an open state, in order to remove the ingredient facilitating the pyrolysis of the fluorine compound of the processing liquid from an atmosphere surrounding the processing chamber. ### Claim 8 (depends on 3) The supercritical processing method as claimed in claim 3, wherein the inert gas is nitrogen gas having a dew point of −50° C. or lower. ### Claim 9 (depends on 4) The supercritical processing method as claimed in claim 4, wherein the fluorine compound includes at least one hydrofluoro ether selected from the group consisting of 1,1,2,2-tetrafluoro-1-(2,2,2-trifluoroethoxy)ethane, 1,1,2,3,3,3-hexafluoro-1-(2,2,2-trifluoroethoxy)propane, and 2,2,3,3,3-pentafluoro-1-(1,1,2,3,3,3-hexafluoropropoxy)propane.