# US 2021/0340674 A1 · Quartz crystal microbalance concentration monitor

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- Number: US 2021/0340674 A1
- Document ID: US20210340674A1
- Status: Published application
- Kind: A1
- Application number: 16/864,877
- Filed: 2020-05-01
- Published: 2021-11-04
- Earliest claimed: 2020-05-01
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Jereld Winkler; Mohith Verghese
- Web page: https://patentgrep.com/patent/US20210340674A1

## CPC

- C23C 16/52: Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)}
- C23C 16/4408: {by purging residual gases from the reaction chamber or gas lines}
- C23C 16/448: characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C 16/45544: {characterized by the apparatus}
- C23C 16/45561: {Gas plumbing upstream of the reaction chamber}
- H10P 14/6339: {deposition by cyclic CVD, e.g. ALD, ALE or pulsed CVD}
- H10P 74/238: {comprising acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection or in-situ thickness measurement}
- 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)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

Describe is a quartz crystal microbalance (QCM) device mounted within a heated sample chamber. The sample chamber temperature is maintained about 10° C. to about 30° C. greater than the temperature of the precursor vessel. The sample chamber is connected to the precursor delivery line and includes a high temperature valve and a flow pathway to foreline with a high temperature valve to permit removal of excess material. The QCM device includes a heater and gas cooling channel allowing the device to be maintained at a temperature about 10° C. to about 30° C. less than the temperature of the precursor vessel.

## Claims

### Claim 1

A processing system comprising:
a carrier gas source;
a precursor vessel;
a deposition chamber; and
a sample chamber downstream of the precursor vessel and upstream of the deposition chamber, the sample chamber housing a quartz crystal microbalance (QCM) device.

### Claim 2 (depends on 1)

The processing system of claim 1, wherein the deposition chamber is selected from one or more of an atomic layer deposition (ALD) chamber, or a chemical vapor deposition (CVD) chamber.

### Claim 3 (depends on 1)

The processing system of claim 1, further comprising a heater and a gas cooling channel within the sample chamber.

### Claim 4 (depends on 1)

The processing system of claim 1, wherein the carrier gas source comprises a carrier gas selected from one or more of argon (Ar), helium (He), xenon (Xe), hydrogen (H2), and nitrogen (N2).

### Claim 5 (depends on 1)

The processing system of claim 1, wherein the quartz crystal microbalance (QCM) device comprises one or more of a sensor head, a crystal holder, a crystal, a feedthrough, an oscillator, and a frequency counter.

### Claim 6 (depends on 5)

The processing system of claim 5, wherein the crystal comprises one or more of an AT crystal or a RC crystal.

### Claim 7 (depends on 5)

The processing system of claim 5, comprising a range of from 1 to 24 crystals.

### Claim 8 (depends on 1)

The processing system of claim 1, further comprising a controller.

### Claim 9 (depends on 8)

The processing system of claim 8, wherein the controller comprises one or more of a central processing unit (CPU), a memory, circuits, and an input/output.

### Claim 10 (depends on 1)

The processing system of claim 1, further comprising a purge gas source and a reservoir, the reservoir downstream of the precursor vessel and the sample chamber and upstream of the deposition chamber.

### Claim 11 (depends on 10)

The processing system of claim 10, wherein the purge gas source comprises a purge gas selected from one or more of argon (Ar), helium (He), xenon (Xe), hydrogen (H2), and nitrogen (N2).

### Claim 12 (depends on 1)

The processing system of claim 1, wherein the vessel is an ampoule.

### Claim 13 (depends on 1)

The processing system of claim 1, wherein the precursor is selected from one or more of a solid precursor or a liquid precursor.

### Claim 14

A processing method comprising:
heating a vessel containing a chemical precursor to a temperature in a range of from about 10° C. to about 600° C., the vessel having a first precursor concentration;
flowing a carrier gas through the vessel to form a precursor gas comprising the chemical precursor;
measuring a concentration of the chemical precursor within the precursor gas using a quartz crystal microbalance (QCM) device within a sample chamber, the precursor having a second precursor concentration, and the sample chamber having a temperature in a range of from about 10° C. to about 30° C. greater than the temperature of the vessel;
exposing a substrate to the precursor gas during a deposition process; and
depositing a film on the substrate.

### Claim 15 (depends on 14)

The processing method of claim 14, wherein heating the vessel vaporizes the chemical precursor.

### Claim 16 (depends on 14)

The processing method of claim 14, wherein the quartz crystal microbalance (QCM) device has a temperature in a range of from about 10° C. to about 15° C. less than the temperature of the vessel.

### Claim 17 (depends on 14)

The processing method of claim 14, wherein the measuring the concentration of the chemical precursor within the precursor gas is conducted in a time frame of about 50 milliseconds to about 20 seconds.

### Claim 18

A non-transitory computer readable medium including instructions, that, when executed by a controller of a processing system, causes the processing system to perform operations of:
heat a vessel containing a chemical precursor to a temperature in a range of from about 25° C. to about 600° C.;
flow a carrier gas through the vessel to form a precursor gas comprising the chemical precursor;
measure a concentration of the chemical precursor within the precursor gas using a quartz crystal microbalance (QCM) within a sample chamber, the sample chamber having a temperature in a range of from about 10° C. to about 30° C. greater than the temperature of the vessel;
expose a substrate to the precursor gas during a deposition process; and
deposit a film on the substrate.

### Claim 19 (depends on 18)

The non-transitory computer readable medium of claim 18, wherein the quartz crystal microbalance (QCM) device has a temperature in a range of from about 10° C. to about 30° C. less than the temperature of the vessel.

### Claim 20 (depends on 18)

The non-transitory computer readable medium of claim 18, wherein the measuring the concentration of the chemical precursor within the precursor gas is conducted in a time frame of less than about 100 milliseconds.
