# US 2021/0341384 A1 · Determination method and treatment method

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- Number: US 2021/0341384 A1
- Document ID: US20210341384A1
- Status: Published application
- Kind: A1
- Application number: 17/305,473
- Filed: 2021-07-08
- Published: 2021-11-04
- Earliest claimed: 2019-01-25
- Assignees: Kabushiki Kaisha Toshiba; Kioxia Corporation; Tohoku University
- Applicants: Kabushiki Kaisha Toshiba; Kioxia Corporation; Tohoku University
- Inventors: Kenya UCHIDA; Hiroyuki FUKUI; Ikuo UEMATSU; Takeaki IWAMOTO; Eunsang KWON
- Web page: https://patentgrep.com/patent/US20210341384A1

## CPC

- G01N 21/3563: for analysing solids; Preparation of samples therefor
- C01B 33/107: Halogenated silanes
- C23C 16/44: characterised by the method of coating (C23C16/04 takes precedence)
- G01N 21/65: Raman scattering
- G01N 24/088: {Assessment or manipulation of a chemical or biochemical reaction, e.g. verification whether a chemical reaction occurred or whether a ligand binds to a receptor in drug screening or assessing reaction kinetics}
- G01R 33/46: NMR spectroscopy
- H10P 14/60: of insulating materials
- C30B 25/02: Epitaxial-layer growth
- G01N 21/35: using infrared light (G01N21/39 takes precedence)
- G01N 2021/8411: {Application to online plant, process monitoring}
- G01N 2201/06113: Coherent sources; lasers
- 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)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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)
- G01R: MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES (indicating correct tuning of resonant circuits H03J3/12)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR

## Abstract

According to one embodiment, a determination method is provided. The determination method determines progress of a treatment of a side-product produced in a process of reacting a substance containing a halogen and silicon or reacting a substance containing silicon and a substance containing a halogen. The treatment of the side-product includes bringing the side-product into contact with a treatment fluid containing water to obtain a first solid matter. The determination method includes determining the progress of the treatment of the side-product based on a signal according to a chemical analysis of at least one of an Si-α bond (α is at least one selected from the group consisting of F, Cl, Br, and I) and an Si—H bond, of the first solid matter.

## Claims

### Claim 1

A determination method for determining progress of a treatment of a side-product produced in a process of reacting a substance containing a halogen and silicon or reacting a substance containing silicon and a substance containing a halogen,
the treatment of the side-product comprising bringing the side-product into contact with a treatment fluid containing water to obtain a first solid matter,
the determination method comprising determining the progress of the treatment of the side-product based on a signal according to a chemical analysis of at least one of an Si-α bond (α is at least one selected from the group consisting of F, Cl, Br, and I) and an Si—H bond, of the first solid matter.

### Claim 2 (depends on 1)

The determination method according to claim 1, comprising determining that the treatment of the side-product has completed when an intensity of the signal is equal to or less than a threshold value, and determining that the treatment of the side-product has not completed when the intensity of the signal exceeds the threshold value.

### Claim 3 (depends on 1)

The determination method according to claim 1, wherein the chemical analysis is an infrared spectroscopic analysis.

### Claim 4 (depends on 2)

The determination method according to claim 2, wherein the chemical analysis is an infrared spectroscopic analysis.

### Claim 5 (depends on 3)

The determination method according to claim 3, comprising:
determining that the treatment of the side-product has completed when an absorbance I1 of a local maximum value in a range of a wavenumber of 800 cm−1 or more and 900 cm−1 or less, in an infrared spectrum of the first solid matter, is 0.050 or less;
determining that part of the treatment of the side-product has not completed when the absorbance I1 of the local maximum value is more than 0.050 and 0.10 or less; and
determining that the treatment of the side-product has not completed when the absorption I1 of the local maximum value is more than 0.10.

### Claim 6 (depends on 4)

The determination method according to claim 4, comprising:
determining that the treatment of the side-product has completed when an absorbance I1 of a local maximum value in a range of a wavenumber of 800 cm−1 or more and 900 cm−1 or less, in an infrared spectrum of the first solid matter, is 0.050 or less;
determining that part of the treatment of the side-product has not completed when the absorbance I1 of the local maximum value is more than 0.050 and 0.10 or less; and
determining that the treatment of the side-product has not completed when the absorption TI of the local maximum value is more than 0.10.

### Claim 7 (depends on 3)

The determination method according to claim 3, comprising:
determining that the treatment of the side-product has completed when a value (I1-I2) where, from an absorbance I1 of a local maximum value in a range of a wavenumber 800 cm−1 or more and 900 cm−1 or less, is subtracted an absorbance I2 of a local minimum value in a range of a wavenumber of 900 cm−1 or more and 1000 cm−1 or less and located at a higher wavenumber side than the local maximum value, in an infrared spectrum of the first solid matter, is 0.001 or less;
determining that part of the treatment of the side-product has not completed when the value (I1-I2) is more than 0.001 and the absorption I2 of the local minimum value is 0.130 or less; and
determining that the treatment of the side-product has not completed when the value (I1-I2) is more than 0.001 and the absorbance I2 of the local minimum value is more than 0.130.

### Claim 8 (depends on 4)

The determination method according to claim 4, comprising:
determining that the treatment of the side-product has completed when a value (I1-I2) where, from an absorbance I1 of a local maximum value in a range of a wavenumber 800 cm−1 or more and 900 cm−1 or less, is subtracted an absorbance I2 of a local minimum value in a range of a wavenumber of 900 cm−1 or more and 1000 cm−1 or less and located at a higher wavenumber side than the local maximum value, in an infrared spectrum of the first solid matter, is 0.001 or less;
determining that part of the treatment of the side-product has not completed when the value (I1-I2) is more than 0.001 and the absorption I2 of the local minimum value is 0.130 or less; and
determining that the treatment of the side-product has not completed when the value (I1-I2) is more than 0.001 and the absorbance I2 of the local minimum value is more than 0.130.

### Claim 9 (depends on 1)

The determination method according to claim 1, wherein the chemical analysis is a Raman spectroscopic analysis.

### Claim 10 (depends on 2)

The determination method according to claim 2, wherein the chemical analysis is a Raman spectroscopic analysis.

### Claim 11 (depends on 9)

The determination method according to claim 9, comprising:
determining that the treatment of the side-product has completed, when a ratio R1/R2 between an intensity R1 of a first local maximum value in a range of a Raman shift of 2000 cm−1 or more and 2500 cm−1 or less and an intensity R2 of a second local maximum value in a range of a Raman shift of 2700 cm−1 or more and 3500 cm−1 or less, in a Raman spectrum of the first solid matter, is 1/5 or less; and
determining that the treatment of the side-product has not completed when the ratio R1/R2 is greater than 1/5.

### Claim 12 (depends on 10)

The determination method according to claim 10, comprising:
determining that the treatment of the side-product has completed, when a ratio R1/R2 between an intensity R1 of a first local maximum value in a range of a Raman shift of 2000 cm−1 or more and 2500 cm−1 or less and an intensity R2 of a second local maximum value in a range of a Raman shift of 2700 cm−1 or more and 3500 cm−1 or less, in a Raman spectrum of the first solid matter, is 1/5 or less; and
determining that the treatment of the side-product has not completed when the ratio R1/R2 is greater than 1/5.

### Claim 13 (depends on 1)

The determination method according to claim 1, wherein the chemical analysis is a nuclear magnetic resonance spectroscopic analysis.

### Claim 14 (depends on 2)

The determination method according to claim 2, wherein the chemical analysis is a nuclear magnetic resonance spectroscopic analysis.

### Claim 15

A treatment method for treating a side-product produced in a process of reacting a substance containing a halogen and silicon or reacting a substance containing silicon and a substance containing a halogen, the method comprising:
bringing the side-product into contact with a treatment fluid containing water to obtain a first solid matter; and
determining progress of treatment of the side-product based on a signal according to a chemical analysis of at least one of an Si-α bond (α is at least one selected from the group consisting of F, Cl, Br, and I) and an Si—H bond, of the first solid matter.

### Claim 16 (depends on 15)

The treatment method according to claim 15, wherein the treatment fluid is a basic aqueous solution.

### Claim 17 (depends on 15)

The treatment method according to claim 15, comprising discontinuing the treatment of the side-product when an intensity of the signal is equal to or less than a threshold value, and further adding more of the treatment fluid to a mixture of the first solid matter and the treatment fluid when the intensity of the signal exceeds the threshold value.

### Claim 18 (depends on 16)

The treatment method according to claim 16, comprising discontinuing the treatment of the side-product when an intensity of the signal is equal to or less than a threshold value, and further adding more of the treatment fluid to a mixture of the first solid matter and the treatment fluid when the intensity of the signal exceeds the threshold value.

### Claim 19

A treatment method for treating a side-product produced in a process of reacting a substance containing a halogen and silicon or reacting a substance containing silicon and a substance containing a halogen, the method comprising:
bringing the side-product into contact with water to obtain a second solid matter;
bringing the second solid matter into contact with a basic aqueous solution to obtain a third solid matter; and
determining progress of treatment of the side-product based on a signal according to a chemical analysis of at least one of an Si-α bond (α is at least one selected from the group consisting of F, Cl, Br, and I) and an Si—H bond, of the third solid matter.

### Claim 20 (depends on 19)

The treatment method according to claim 19, comprising bringing the second solid matter into contact with the basic aqueous solution based on a signal according to a chemical analysis of at least one of an Si-α bond (α is at least one selected from the group consisting of F, Cl, Br, and I) and a Si—H bond, of the second solid matter.