# US 11,439,967 B2 · Chemical liquid preparation method, chemical liquid preparation device, and substrate processing device

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- Number: US 11,439,967 B2
- Document ID: US11439967B2
- Status: Granted
- Kind: B2
- Application number: 16/114,253
- Filed: 2018-08-28
- Published: 2019-03-28
- Granted: 2022-09-13
- Earliest claimed: 2017-09-22
- Assignees: SCREEN Holdings Co., Ltd.
- Applicants: SCREEN Holdings Co., Ltd.
- Inventors: Hajime Nishide; Takashi Izuta; Takatoshi Hayashi; Katsuhiro Fukui; Koichi Okamoto; Kazuhiro Fujita; Atsuyasu Miura; Kenji Kobayashi; Sei Negoro; Hiroki Tsujikawa
- Web page: https://patentgrep.com/patent/US11439967B2

## CPC

- B01F 35/82: by adding a material to be mixed to a mixture in response to a detected feature, e.g. density, radioactivity, consumed power or colour
- B01F 23/231: by bubbling (mixers with gas or liquid agitation, e.g. with air supply tubes B01F33/40)
- B01F 23/237611: {Air}
- B01F 23/237612: {Oxygen}
- B01F 23/23765: {Nitrogen}
- B01F 35/2132: {Concentration, pH, pOH, p(ION) or oxygen-demand (B01F35/2133 takes precedence)}
- B01F 35/2202: {Controlling the mixing process by feed-back, i.e. a measured parameter of the mixture is measured, compared with the set-value and the feed values are corrected}
- G05D 11/00: Control of flow ratio (control of chemical or physico-chemical variables, e.g. pH-value, G05D21/00; control of humidity G05D22/00; control of temperature by varying the mixing ratio of two fluids having different temperatures G05D23/13; control of viscosity G05D24/00)
- G05D 21/02: characterised by the use of electric means
- H10P 50/644: {Anisotropic liquid etching (H10P50/61 takes precedence)}
- H10P 50/667: {by liquid etching only}
- 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 72/0414: {using mainly spraying means, e.g. nozzles}
- H10P 72/0422: {for wet etching}
- H10P 72/0424: {using mainly spraying means, e.g. nozzles}
- B01F 2101/58: Mixing semiconducting materials, e.g. during semiconductor or wafer manufacturing processes
- B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06)
- G05D: SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

A chemical liquid preparation method of preparing a chemical liquid for treating a film formed on a substrate, including a gas dissolving process in which an oxygen-containing gas and an inert-gas-containing gas are dissolved in the chemical liquid by supplying the oxygen-containing gas which contains oxygen gas and the inert-gas-containing gas which contains an inert gas to a chemical liquid, wherein in the gas dissolving process, a dissolved oxygen concentration in the chemical liquid is adjusted by setting a mixing ratio between the oxygen-containing gas and the inert-gas-containing gas supplied to the chemical liquid as a mixing ratio corresponding to a predetermined target dissolved oxygen concentration.

## Claims

### Claim 1

A chemical liquid preparation method of preparing a chemical liquid to be supplied to a substrate, comprising:
a setting step of setting a mixing ratio of an oxygen-containing gas and an inert-gas-containing gas corresponding to a predetermined target dissolved oxygen concentration in the chemical liquid;
an operating step of operating a first flow rate adjusting valve to supply the oxygen-containing gas with a first supply flow rate from an oxygen-containing gas piping to a mixed gas piping and operating a second flow rate adjusting valve to supply the inert-gas-containing gas with a second supply flow rate from an inert-gas-containing gas piping to the mixed gas piping, wherein a ratio of the first supply flow rate and the second supply flow rate is corresponding to the set mixing ratio, so as to produce a mixed gas of the oxygen-containing gas and the inert-gas-containing gas in the mixed gas piping; and
a gas dissolving step of supplying the mixed gas from the mixed gas piping into the chemical liquid and dissolving the mixed gas in the chemical liquid so as to adjust a dissolved oxygen concentration to the predetermined target dissolved oxygen concentration.

### Claim 2 (depends on 1)

The chemical liquid preparation method according to claim 1,
wherein the chemical liquid to be prepared comprises a TMAH-containing chemical liquid which contains tetramethylammonium hydroxide (TMAH).

### Claim 3 (depends on 1)

The chemical liquid preparation method according to claim 1,
wherein the gas dissolving step comprises a process in which bubbles are generated in the chemical liquid by discharging the mixed gas in the chemical liquid.

### Claim 4 (depends on 2)

The chemical liquid preparation method according to claim 2,
wherein the gas dissolving step comprises a process in which bubbles are generated in the chemical liquid by discharging the mixed gas in the chemical liquid.

### Claim 5 (depends on 1)

The chemical liquid preparation method according to claim 1,
wherein the chemical liquid to be subjected to the gas dissolving step comprises a chemical liquid recovered from a processing unit.

### Claim 6

A chemical liquid preparation method of preparing a chemical liquid to be supplied to a substrate, comprising:
a first operating step of operating a first flow rate adjusting valve to supply an oxygen-containing gas with a first supply flow rate from a first oxygen-containing gas piping to a first mixed gas piping and operating a second flow rate adjusting valve to supply an inert-gas-containing gas with a second supply flow rate from a first inert-gas-containing gas piping to the first mixed gas piping, wherein a ratio of the first supply flow rate and the second supply flow rate in the first operating step is corresponding to a first predetermined mixing ratio, so as to produce a first mixed gas of the oxygen-containing gas and the inert-gas-containing gas in the first mixed gas piping;
a first gas dissolving step of supplying the first mixed gas from the first mixed gas piping into the chemical liquid and dissolving the first mixed gas in the chemical liquid so as to adjust a dissolved oxygen concentration in the chemical liquid;
a second operating step of operating a third flow rate adjusting valve to supply the oxygen-containing gas with a third supply flow rate from a second oxygen-containing gas piping to a second mixed gas piping and operating a fourth flow rate adjusting valve to supply the inert-gas-containing gas with a fourth supply flow rate from a second inert-gas-containing gas piping to the second mixed gas piping, wherein a ratio of the third supply flow rate and the fourth supply flow rate in the second operating step is corresponding to a second predetermined mixing ratio which corresponds to a predetermined target dissolved oxygen concentration in the chemical liquid, so as to produce a second mixed gas of the oxygen-containing gas and the inert-gas-containing gas in the second mixed gas piping;
a second gas dissolving step of, after the first gas dissolving step, supplying the second mixed gas from the second mixed gas piping into the chemical liquid and dissolving the second mixed gas in the chemical liquid so as to further adjust the dissolved oxygen concentration in the chemical liquid whose oxygen concentration has been adjusted by the first gas dissolving step.

### Claim 7 (depends on 6)

The chemical liquid preparation method according to claim 6,
wherein the first predetermined mixing ratio is the same as the second predetermined mixing ratio.

### Claim 8 (depends on 6)

The chemical liquid preparation method according to claim 6,
wherein, the first predetermined mixing ratio is lower in the oxygen-containing gas ratio than the second predetermined mixing ratio.

### Claim 9 (depends on 1)

The chemical liquid preparation method according to claim 1, further comprising
a measurement step in which a dissolved oxygen concentration of the chemical liquid after gas is dissolved by the gas dissolving step is measured;
an inert gas dissolving step in which, when the dissolved oxygen concentration measured in the measurement step is higher than the target dissolved oxygen concentration, the inert-gas-containing gas is dissolved in the chemical liquid obtained after gas is dissolved by the gas dissolving step by supplying the inert-gas-containing gas to the chemical liquid obtained after gas is dissolved by the gas dissolving step; and
an oxygen-containing gas dissolving step in which, when the dissolved oxygen concentration measured in the measurement step is lower than the target dissolved oxygen concentration, the oxygen-containing gas is dissolved in the chemical liquid obtained after gas is dissolved by the gas dissolving step by supplying the oxygen-containing gas to the chemical liquid obtained after gas is dissolved by the gas dissolving step.
