# US 2022/0044928 A1 · Silicon compounds and methods for depositing films using same

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- Number: US 2022/0044928 A1
- Document ID: US20220044928A1
- Status: Published application
- Kind: A1
- Application number: 17/510,962
- Filed: 2021-10-26
- Published: 2022-02-10
- Earliest claimed: 2019-06-18
- Assignees: Versum Materials US, LLC
- Applicants: Versum Materials US, LLC
- Inventors: ROBERT G. RIDGEWAY; JENNIFER LYNN ANNE ACHTYL; RAYMOND N. VRTIS; XINJIAN LEI; WILLIAM ROBERT ENTLEY
- Web page: https://patentgrep.com/patent/US20220044928A1

## CPC

- H10P 14/6682: {the compound being a silane, e.g. disilane, methylsilane or chlorosilane}
- H10P 14/6922: {the material containing Si, O and at least one of H, N, C, F or other non-metal elements, e.g. SiOC, SiOC:H or SiONC}
- C07F 7/0834: {Compounds having one or more O-Si linkage (for compounds with C-O-Si linkages see C07F7/18)}
- C23C 16/401: {containing silicon}
- C23C 16/448: characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C 16/50: using electric discharges {(generation and control of plasma in discharge tubes for surface treatment H01J37/32, H01J37/34)}
- C23C 16/56: After-treatment
- H10P 14/6336: {in the presence of a plasma [PECVD]}
- H10P 14/6538: {by exposure to UV light}
- H10P 14/6539: {by exposure to corpuscular radiation, e.g. exposure to electrons, alpha-particles, protons or ions}
- H10P 14/6686: {the compound being a molecule comprising at least one silicon-oxygen bond and the compound having hydrogen or an organic group attached to the silicon or oxygen, e.g. a siloxane}
- H10P 14/69215: {the material being a silicon oxide, e.g. SiO2}
- B05D 1/62: {Plasma-deposition of organic layers (plasma deposition in general C23C14/00, C23C16/00)}
- B05D 3/067: {Curing or cross-linking the coating}
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- 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)
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)

## Abstract

A chemical vapor deposition method for producing a dielectric film, the method comprising: providing a substrate into a reaction chamber; introducing gaseous reagents into the reaction chamber wherein the gaseous reagents comprise a silicon precursor comprising an silicon compound having Formula I as defined herein and applying energy to the gaseous reagents in the reaction chamber to induce reaction of the gaseous reagents to deposit a film on the substrate. The film as deposited is suitable for its intended use without an optional additional cure step applied to the as-deposited film.

## Claims

### Claim 1

A chemical vapor deposition method for producing a dielectric film, the method comprising:
providing a substrate into a reaction chamber;
introducing gaseous reagents into the reaction chamber wherein the gaseous reagents comprise a silicon precursor comprising a silicon compound having the following Formula I:
wherein X and Y are independently selected from the group consisting of OR1, OR2, and OC(O)R3; R1-3 are independently selected from the group consisting of a linear or branched C1 to C10 alkyl group, a linear or branched C2 to C10 alkenyl group, a linear or branched C2 to C10 alkynyl group, a C3 to C10 cyclic alkyl group, a C3 to C10 hetero-cyclic alkyl group, a C5 to C10 aryl group, and a C3 to C10 hetero-aryl group; and R4 is a C3 to C5 alkyl di-radical which forms a four-membered, five-membered, or six-membered saturated cyclic ring with the Si atom, and optionally at least one oxygen source; and
applying energy to the gaseous reagents in the reaction chamber to induce reaction of the gaseous reagents to deposit a film on the substrate.

### Claim 2 (depends on 1)

The method of claim 1 wherein the silicon precursor further comprises a hardening additive.

### Claim 3 (depends on 1)

The method of claim 1 wherein the silicon compound comprises at least one selected from the group consisting of 1,1-dimethoxy-1-silacyclopentane, 1,1-diethoxy-1-silacyclopentane, 1,1-di-n-propyloxy-1-silacyclopentane, 1,1-di-iso-propyloxy-1-silacyclopentane, 1,1-dimethoxy-1-silacyclobutane, 1,1-diethoxy-1-silacyclobutane, 1,1-di-n-propyloxy-1-silacyclobutane, 1,1-di-iso-propyloxy-1-silacyclobutane, 1,1-dimethoxy-1-silacyclohexane, 1,1-di-iso-propyloxy-1-silacyclohexane, 1,1-di-n-propyloxy-1-silacyclohexane, 1-methoxy-1-acetoxy-1-silacyclopentane, 1,1-diacetoxy-1-silacyclopentane, 1-methoxy-1-acetoxy-1-silacyclobutane, 1,1-diacetoxy-1-silacyclobutane, 1-methoxy-1-acetoxy-1-silacyclohexane, 1,1-diacetoxy-1-silacyclohexane, 1-ethoxy-1-acetoxy-1-silacyclopentane, 1-ethoxy-1-acetoxy-1-silacyclobutane, and combinations thereof.

### Claim 4 (depends on 2)

The method of claim 2 wherein the hardening additive comprises tetraethoxysilane.

### Claim 5 (depends on 2)

The method of claim 2 wherein the hardening additive comprises tetramethoxysilane.

### Claim 6 (depends on 1)

The method of claim 1 which is a plasma enhanced chemical vapor deposition method.

### Claim 7 (depends on 1)

The method of claim 1 where the optionally at least one oxygen source is selected from the group consisting of O2, N2O, NO, NO2, CO2, water, H2O2, and ozone.

### Claim 8 (depends on 1)

The method of claim 1 where the reaction chamber in the applying step comprises at least one gas selected from the group consisting of He, Ar, N2, Kr, Xe, NH3, H2, CO2, or CO.

### Claim 9 (depends on 1)

The method of claim 1 further comprising a step of applying additional energy to the film.

### Claim 10 (depends on 9)

The method of claim 9 wherein the additional energy is at least one selected from the group consisting of a thermal treatment, an ultraviolet (UV) treatment, an electron beam treatment, and a gamma radiation treatment.

### Claim 11 (depends on 10)

The method of claim 10 wherein the UV treatment occurs during at least a portion of the thermal treatment.

### Claim 12 (depends on 1)

The method of claim 1 wherein the silicon compound included in the gaseous reagents includes less than 100 ppm of any halide ion impurities.

### Claim 13 (depends on 1)

The method of claim 1 wherein the silicon compound included in the gaseous reagents includes less than 5 ppm of any metal ion impurities.

### Claim 14

A chemical vapor deposition method for producing a porous dielectric film, comprising:
providing a substrate into a reaction chamber;
introducing gaseous reagents into the reaction chamber wherein the gaseous reagents comprise a silicon precursor comprising a silicon compound having the following Formula I:
wherein X and Y are independently selected from the group consisting of OR1, OR2, and OC(O)R3; R1-3 are independently selected from the group consisting of a linear or branched C1 to C10 alkyl group, a linear or branched C2 to C10 alkenyl group, a linear or branched C2 to C10 alkynyl group, a C3 to C10 cyclic alkyl group, a C3 to C10 hetero-cyclic alkyl group, a C5 to C10 aryl group, and a C3 to C10 hetero-aryl group; and R4 is a C3 to C5 alkyl di-radical which forms a four-membered, five-membered, or six-membered saturated cyclic ring with the Si atom, and further optionally comprise at least one oxygen source; and
applying energy to the gaseous reagents in the reaction chamber to induce reaction of the gaseous reagents to deposit a film on the substrate.

### Claim 15 (depends on 14)

The method of claim 14 wherein the optional oxygen source is at least one selected from the group consisting of O2, N2O, NO, NO2, CO2, water, H2O2, and ozone.

### Claim 16 (depends on 14)

The method of claim 14 wherein the silicon compound comprises at least one selected from the group consisting of 1,1-dimethoxy-1-silacyclopentane, 1,1-diethoxy-1-silacyclopentane, 1,1-di-n-propyloxy-1-silacyclopentane, 1,1-di-iso-propyloxy-1-silacyclopentane, 1,1-dimethoxy-1-silacyclobutane, 1,1-diethoxy-1-silacyclobutane, 1,1-di-n-propyloxy-1-silacyclobutane, 1,1-di-iso-propyloxy-1-silacyclobutane, 1,1-dimethoxy-1-silacyclohexane, 1,1-di-iso-propyloxy-1-silacyclohexane, 1,1-di-n-propyloxy-1-silacyclohexane, 1-methoxy-1-acetoxy-1-silacyclopentane, 1,1-diacetoxy-1-silacyclopentane, 1-methoxy-1-acetoxy-1-silacyclobutane, 1,1-diacetoxy-1-silacyclobutane, 1-methoxy-1-acetoxy-1-silacyclohexane, 1,1-diacetoxy-1-silacyclohexane, 1-ethoxy-1-acetoxy-1-silacyclopentane, 1-ethoxy-1-acetoxy-1-silacyclobutane, and combinations thereof.

### Claim 17 (depends on 14)

The method of claim 14 wherein the silicon precursor included in the gaseous reagents includes less than 100 ppm of any halide ion impurities.

### Claim 18 (depends on 14)

The method of claim 14 wherein the silicon precursor included in the gaseous reagents includes less than 5 ppm of any metal ion impurities.