# US 11,441,974 B2 · Detection of surface particles on chamber components with carbon dioxide

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- Number: US 11,441,974 B2
- Document ID: US11441974B2
- Status: Granted
- Kind: B2
- Application number: 16/529,630
- Filed: 2019-08-01
- Published: 2021-02-04
- Granted: 2022-09-13
- Earliest claimed: 2019-08-01
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Changgong Wang; Zhili Zuo; Chang Ke; Song-Moon Suh
- Web page: https://patentgrep.com/patent/US11441974B2

## CPC

- G01N 1/02: Devices for withdrawing samples {(sampling of foundation soil E02D1/04; collecting or conveying radioactive samples G01T7/00, e.g. G01T7/02, G01T7/08)}
- G01N 15/02: Investigating particle size or size distribution (by measuring osmotic pressure G01N7/10; investigating sedimentation of particle suspensions G01N15/04; investigating individual particles G01N15/10)
- G01N 15/065: {using condensation nuclei counters}
- G01N 15/14: Optical investigation techniques, e.g. flow cytometry
- G01N 2001/028: {Sampling from a surface, swabbing, vaporising}
- G01N 2015/0019: {Means for transferring or separating particles prior to analysis, e.g. hoppers or particle conveyors}
- G01N 2015/0294: {Particle shape}
- G01N 2015/1493: {Particle size}
- G01N 2015/1497: {Particle shape}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

Disclosed herein is a method comprising directing, from a distribution unit, a stream comprising at least one of solid CO2 particles or CO2 droplets toward an article, wherein the article comprises a plurality of surface particles, and wherein the stream comprising at least one of solid CO2 particles or CO2 droplets causes at least a portion of the plurality of surface particles on the article to dislodge from the surface of the article; collecting, on a surface of a substrate having a pre-determined initial state comprising initial surface particles on the surface of the substrate or a real-time aerosol sampling unit, at least some of the portion of the plurality of surface particles dislodged from the surface of the article; analyzing the surface of the substrate after performing the collecting; and determining at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of the portion of the plurality of surface particles that were dislodged from the surface of the article and collected on the surface of the substrate.

## Claims

### Claim 1

A method comprising:
directing, from a distribution unit, a stream comprising at least one of solid CO2 particles or CO2 droplets toward an article, wherein the article comprises a plurality of surface particles, and wherein the stream comprising at least one of solid CO2 particles or CO2 droplets causes at least a portion of the plurality of surface particles on the article to dislodge from a surface of the article;
collecting, on a surface of a substrate having a pre-determined initial state comprising initial surface particles on the surface of the substrate, at least some of the portion of the plurality of surface particles dislodged from the surface of the article;
analyzing the initial surface particles and the collected particles of the plurality of surface particles on the surface of the substrate after performing the collecting; and
determining, based on the analysis of the initial surface particles and the collected particles of the plurality of surface particles, at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of the portion of the plurality of surface particles that were dislodged from the surface of the article and collected on the surface of the substrate.

### Claim 2 (depends on 1)

The method of claim 1, further comprising:
determining information about at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of a remainder of the plurality of surface particles on the article.

### Claim 3 (depends on 1)

The method of claim 1, wherein determining at least one of the size, the morphology, the chemical composition, the particle number concentration, or the particle size distribution of the portion of the plurality of surface particles that were dislodged from the surface of the article and collected on the surface of the substrate comprises:
determining at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of all detectable surface particles on the substrate; and
subtracting out at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of pre-determined particles included in the pre-determined initial state;
wherein a remainder of at least one of the size, the morphology, the chemical composition, the particle number concentration, or the particle size distribution of all detectable surface particles on the substrate represents data for the portion of the plurality of surface particles that were dislodged from the surface of the article and collected on the surface of the substrate.

### Claim 4 (depends on 1)

The method of claim 1, further comprising:
generating a laminar flow around the article to transport the portion of the plurality of surface particles dislodged from the surface of the article to the substrate.

### Claim 5 (depends on 1)

The method of claim 1, further comprising:
reducing, by one or more particle charge neutralizers, a charge of the portion of the plurality of surface particles dislodged from the surface of the article such to facilitate transport to the substrate.

### Claim 6 (depends on 1)

The method of claim 1, wherein directing the stream comprising at least one of solid CO2 particles or CO2 droplets toward the article comprises:
forming a first layer of solid CO2 on the surface of the article, wherein the first layer of solid CO2 causes the portion of the plurality of surface particles to be dislodged from the surface of the article, and wherein at least a portion of the dislodged surface particles are to collect on the surface of the article;
increasing a temperature of the article to facilitate sublimation of the first layer of solid CO2; and
forming a second layer of solid CO2 on the surface of the article, wherein the second layer of solid CO2 causes the portion of the dislodged surface particles to be dislodged from the surface of the article.

### Claim 7 (depends on 1)

The method of claim 1, wherein directing the stream comprising at least one of solid CO2 particles or CO2 droplets towards the article comprises:
flowing liquid CO2 into the distribution unit, wherein the liquid CO2 is converted into at least one of solid CO2 particles or CO2 droplets upon exiting the distribution unit.

### Claim 8

An apparatus comprising:
a distribution unit configured to generate a stream comprising at least one of solid CO2 particles or CO2 droplets;
a controller configured to direct the stream comprising at least one of solid CO2 particles or CO2 droplets toward an article comprising a plurality of surface particles, wherein the stream causes at least a portion of the plurality of surface particles on the article to dislodge from a surface of the article;
a laminar flow component configured to generate a laminar flow around the article to transport the portion of the plurality of surface particles that were dislodged from the surface of the article away from the article; and
a substrate having a pre-determined initial state comprising surface particles on a surface of the substrate, wherein a surface of the substrate is to collect the portion of the plurality of surface particles dislodged from the surface of the article, and wherein the surface of the substrate is to be analyzed to determine at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of the portion of the plurality of surface particles that were dislodged from the surface of the article and collected on the surface of the substrate.

### Claim 9 (depends on 8)

The apparatus of claim 8, wherein information about at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of a remainder of the plurality of surface particles on the article is determined based on a determination of at least one of a size, a morphology, a chemical composition, a particle number concentration, or a particle size distribution of the portion of the plurality of surface particles that were dislodged from the surface of the article and collected on the surface of the substrate.

### Claim 10 (depends on 8)

The apparatus of claim 8, further comprising one or more particle charge neutralizers configured to reduce a charge of the portion of the plurality of surface particles that were dislodged from the surface of the article such to facilitate transport to the substrate.

### Claim 11 (depends on 8)

The apparatus of claim 8, further comprising a liquid CO2 source fluidly coupled to the distribution unit, wherein liquid CO2 is configured to flow from the liquid CO2 source into the distribution unit such that the liquid CO2 is converted into at least one of solid CO2 particles or CO2 droplets upon exiting the distribution unit.

### Claim 12 (depends on 8)

The apparatus of claim 8, wherein the controller is further configured to:
direct a first stream comprising at least one of solid CO2 particles or CO2 droplets toward the article for a first time period, wherein the first stream causes a first layer of solid CO2 to be formed on the article, and wherein the first layer of solid CO2 causes the portion of the plurality of surface particles to be dislodged from the surface of the article, and wherein at least a portion of the dislodged surface particles are to collect on the surface of the article;
stop the first stream for a second time period during which a temperature of the article is increased to facilitate sublimation of the first layer of solid CO2 on the surface of the article; and
direct a second stream comprising at least one of solid CO2 particles or CO2 droplets toward the article for a third time period, wherein the second stream causes a second layer of solid CO2 to be formed on the article, and wherein the second layer of solid CO2 causes the portion of the dislodged surface particles to be dislodged from the surface of the article.

### Claim 13

An apparatus comprising:
a distribution unit configured to generate one or more streams each comprising at least one of solid CO2 particles or CO2 droplets;
a controller configured to:
direct a first stream comprising at least one of solid CO2 particles or CO2 droplets toward an article comprising a plurality of surface particles for a first time period, wherein the stream causes a first layer of solid CO2 to be formed on the article, and wherein the first layer of solid CO2 causes at least a portion of the plurality of surface particles on the article to dislodge from a surface of the article;
modify a temperature of the article to facilitate sublimation of the first layer of solid CO2 on the surface of the article; and
direct a second stream comprising at least one of solid CO2 particles or solid CO2 droplets towards the article for a second time period, wherein the second stream causes a second layer of solid CO2 to be formed on the article, and wherein the second layer of solid CO2 causes an additional portion of the plurality of surface particles to be dislodged from the surface of the article; and
a real-time aerosol sampling component configured to collect surface particles that are dislodged from the surface of the article, wherein the collected surface particles are to be analyzed to determine, in real-time, at least one of a particle number concentration, a particle size, or a particle size distribution.

### Claim 14 (depends on 13)

The apparatus of claim 13, wherein information about at least one of a size, a particle number concentration, a particle size, or a particle size distribution of a remainder of the plurality of surface particles on the article is determined based on a determination of at least one of a particle number concentration, a particle size, or a particle size distribution of the portion of the plurality of surface particles that were dislodged from the surface of the article and collected by the real-time aerosol sampling component.

### Claim 15 (depends on 13)

The apparatus of claim 13, further comprising a laminar flow component configured to generate a laminar flow around the article to transport the portion of the plurality of surface particles that were dislodged from the surface of the article to the real-time aerosol sampling component.

### Claim 16 (depends on 13)

The apparatus of claim 13, further comprising one or more particle charge neutralizers configured to reduce a charge of the portion of the plurality of surface particles that were dislodged from the surface of the article such to facilitate transport to the real-time aerosol sampling component.

### Claim 17 (depends on 13)

The apparatus of claim 13, further comprising a liquid CO2 source fluidly coupled to the distribution unit, wherein liquid CO2 is configured to flow from the liquid CO2 source into the distribution unit such that the liquid CO2 is converted into at least one of solid CO2 particles or CO2 droplets upon exiting the distribution unit.

### Claim 18 (depends on 13)

The apparatus of claim 13, wherein the article is supported by an article support assembly, and wherein to modify the temperature of the article, the controller is to:
stop the first stream for a third time period between the first time period and the second time period; and
increase a temperature of the article support assembly, wherein increasing the temperature of the article support assembly causes an increase in the temperature of the article.

### Claim 19 (depends on 13)

The apparatus of claim 13, wherein the real-time aerosol sampling component comprises at least one of a laser particle counter, an aerodynamic particle sizer, a condensation particle counter, or an ultrafine condensation particle counter.

### Claim 20 (depends on 13)

The apparatus of claim 13, wherein modifying the temperature of the article comprises:
modifying a temperature of at least one of solid CO2 particles or CO2 droplets directed towards the article, wherein a temperature of the second stream directed towards the article corresponds to the modified temperature.
