# US 10,483,099 B1 · Method for forming thermally stable organosilicon polymer film

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- Number: US 10,483,099 B1
- Document ID: US10483099B1
- Status: Granted
- Kind: B1
- Application number: 16/046,218
- Filed: 2018-07-26
- Granted: 2019-11-19
- Earliest claimed: 2018-07-26
- Assignees: ASM IP Holding B.V.
- Applicants: ASM IP Holding B.V.
- Inventors: Timothee Julien Vincent Blanquart
- Web page: https://patentgrep.com/patent/US10483099B1

## CPC

- C23C 16/045: {Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates}
- H10P 14/683: {carbon-based polymeric organic materials, e.g. polyimides, poly cyclobutene or PVC}
- C23C 16/401: {containing silicon}
- C23C 16/4554: {Plasma being used non-continuously in between ALD reactions (C23C16/56 takes precedence)}
- C23C 16/45542: {Plasma being used non-continuously during the ALD reactions}
- C23C 16/45553: {characterized by the use of precursors specially adapted for ALD}
- C23C 16/505: using radio frequency discharges
- H10P 14/6336: {in the presence of a plasma [PECVD]}
- H10P 14/6339: {deposition by cyclic CVD, e.g. ALD, ALE or pulsed CVD}
- H10P 14/6532: {by exposure to a plasma}
- H10P 14/6682: {the compound being a silane, e.g. disilane, methylsilane or chlorosilane}
- H10P 14/6903: {containing silicon}
- H10P 14/6905: {being a silicon carbide or silicon carbonitride and not containing oxygen, e.g. SiC or SiC:H}
- H10W 10/014: {using trench refilling with dielectric materials, e.g. shallow trench isolations}
- H10W 10/17: formed using trench refilling with dielectric materials, e.g. shallow trench isolations
- 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
- H10W: GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10

## Abstract

A method of forming a thermally stable organosilicon polymer includes: (i) depositing an organosilicon polymer whose backbone is composed of silicon atoms on a substrate using a silicon-containing precursor in a reaction space; and (ii) exposing the organosilicon polymer deposited in step (i) to a hydrogen plasma in the absence of the precursor in the reaction space in a manner increasing Si—H bonds and decreasing C—H bonds in the organosilicon polymer without depositing an organosilicon polymer.

## Claims

### Claim 1

A method of forming a thermally stable organosilicon polymer, comprising:
(i) depositing an organosilicon polymer whose backbone is primarily or partly composed of silicon atoms on a substrate using a silicon-containing precursor in a reaction space; and
(ii) exposing the organosilicon polymer deposited in step (i) to a hydrogen plasma in the absence of the precursor in the reaction space in a manner increasing Si—H bonds and decreasing C—H bonds in the organosilicon polymer without depositing an organosilicon polymer.

### Claim 2 (depends on 1)

The method according to claim 1, wherein step (i) comprises conducting one or more cycles of atomic layer deposition (ALD), and steps (i) and (ii) are repeated as step (iii) until a desired thickness of the organosilicon polymer is obtained.

### Claim 3 (depends on 1)

The method according to claim 1, wherein step (i) comprises conducting chemical vapor deposition (CVD), and steps (i) and (ii) are repeated as step (iii) until a desired thickness of the organosilicon polymer is obtained.

### Claim 4 (depends on 2)

The method according to claim 2, wherein the ALD is plasma-enhanced ALD (PEALD), and step (ii) is conducted 2 to 10 times after conducting each cycle of PEALD.

### Claim 5 (depends on 3)

The method according to claim 3, wherein the CVD is thermal or plasma-enhanced CVD, and step (ii) is conducted after every deposition of the organosilicon polymer having a thickness of 1 to 50 nm in step (i).

### Claim 6 (depends on 1)

The method according to claim 1, wherein step (ii) comprises applying RF power to the reaction space in a range of 0.07 W/cm2 to 1.4 W/cm2 to generate the hydrogen plasma.

### Claim 7 (depends on 1)

The method according to claim 1, wherein step (ii) is conducted for 10 seconds to 60 seconds.

### Claim 8 (depends on 1)

The method according to claim 1, wherein step (ii) comprises supplying hydrogen gas and noble gas to the reaction space at a ratio of hydrogen gas flow to total flow of gases including hydrogen gas and noble gas, which is 0.1 to 0.8.

### Claim 9 (depends on 1)

The method according to claim 1, wherein step (ii) comprises supplying only hydrogen gas to the reaction space to generate the hydrogen plasma.

### Claim 10 (depends on 2)

The method according to claim 2, further comprising, after step (iii), annealing the organosilicon polymer wherein the organosilicon polymer manifests substantially no shrinkage.

### Claim 11 (depends on 1)

The method according to claim 1, wherein the organosilicon polymer is constituted by polysilane, polycarbosilane, polysilazane, or polysiloxane.

### Claim 12 (depends on 1)

The method according to claim 1, wherein in step (ii), the hydrogen plasma is a pulsed plasma generated by applying RF power to the reaction space in pulses.

### Claim 13 (depends on 1)

The method according to claim 1, wherein step (i) and step (ii) are conducted continuously in a same reaction chamber.