# US 12,000,042 B2 · Sequential infiltration synthesis apparatus and a method of forming a patterned structure

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- Number: US 12,000,042 B2
- Document ID: US12000042B2
- Status: Granted
- Kind: B2
- Application number: 17/885,810
- Filed: 2022-08-11
- Published: 2022-12-08
- Granted: 2024-06-04
- Earliest claimed: 2016-12-15
- Assignees: ASM IP Holding B.V.
- Applicants: ASM IP Holding B.V.
- Inventors: Jan Willem Maes; Werner Knaepen; Krzysztof Kamil Kachel; David Kurt De Roest; Bert Jongbloed; Dieter Pierreux
- Web page: https://patentgrep.com/patent/US12000042B2

## CPC

- C23C 16/45523: {Pulsed gas flow or change of composition over time}
- C23C 16/04: Coating on selected surface areas, e.g. using masks
- C23C 16/042: {using masks}
- C23C 16/045: {Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates}
- C23C 16/26: Deposition of carbon only
- C23C 16/4412: {Details relating to the exhausts, e.g. pumps, filters, scrubbers, particle traps}
- C23C 16/448: characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C 16/4485: {by evaporation without using carrier gas in contact with the source material (C23C16/4486 takes precedence)}
- C23C 16/45527: {characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations}
- C23C 16/52: Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)}
- C23C 16/56: After-treatment
- H10P 76/405: {characterised by their composition, e.g. multilayer masks}
- H10P 76/4085: {characterised by the processes involved to create the masks}
- 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

A sequential infiltration synthesis apparatus comprising: a reaction chamber constructed and arranged to hold at least a first substrate; a precursor distribution and removal system to provide to and remove from the reaction chamber a vaporized first or second precursor; and, a sequence controller operably connected to the precursor distribution and removal system and comprising a memory provided with a program to execute infiltration of an infiltrateable material provided on the substrate when run on the sequence controller by: activating the precursor distribution and removal system to provide and maintain the first precursor for a first period T1 in the reaction chamber; activating the precursor distribution and removal system to remove a portion of the first precursor from the reaction chamber for a second period T2; and, activating the precursor distribution and removal system to provide and maintain the second precursor for a third period T3 in the reaction chamber. The program in the memory is programmed with the first period T1 longer than the second period T2.

## Claims

### Claim 1

A sequential infiltration synthesis apparatus comprising:
a reaction chamber constructed and arranged to hold at least a first substrate;
a precursor distribution and removal system to provide to, and remove from the reaction chamber a vaporized first or second precursor; and,
a sequence controller operably connected to the precursor distribution and removal system and comprising a memory provided with a program to execute infiltration of an infiltrateable material provided on the substrate when run on the sequence controller by:
activating the precursor distribution and removal system to provide and maintain the first precursor for a first period T1 in the reaction chamber;
activating the precursor distribution and removal system to remove a portion of the first precursor from the reaction chamber for a second period T2; and
activating the precursor distribution and removal system to provide and maintain the second precursor for a third period T3 in the reaction chamber, wherein the program in the memory is programmed to execute during the first period T1 or third period T3:
activating the precursor distribution and removal system to open a first precursor flow path and close a gas removal flow path and provide the first precursor to the reaction chamber for a load period LP; and
activating the precursor distribution and removal system to close the first precursor flow path and maintain the first precursor in the reaction chamber while keeping the removal flow path closed for a soak period SP.

### Claim 2 (depends on 1)

The apparatus according to claim 1, wherein the program in the memory is programmed to:
activate the precursor distribution and removal system to open the gas removal flow path and provide the first precursor to the reaction chamber simultaneously to flush the first precursor through the reactor for a flush period FP before the load period LP.

### Claim 3 (depends on 1)

The apparatus according to claim 1, wherein the apparatus is provided with a pressure sensor constructed and arranged to measure the pressure in the reaction chamber and operably connected to the sequence flow controller and the program in the memory is programmed to:
terminate the load period LP when the pressure in the reaction chamber reaches the desired process pressure.

### Claim 4 (depends on 1)

A method of forming a patterned structure with the sequential infiltration synthesis apparatus according to claim 1, wherein the method comprises:
providing a substrate with a patterned infiltrateable material in the reaction chamber; and,
infiltrating the patterned infiltrateable material with infiltration material in at least one infiltration cycle.

### Claim 5 (depends on 4)

The method according to claim 4, wherein the substrate comprises a hardmask comprising a spin on glass or spin on carbon between the substrate and the patterned infiltrateable material.

### Claim 6 (depends on 4)

The method according to claim 4, wherein the substrate comprises a hardmask comprising a silicon nitride layer between the substrate and the patterned infiltrateable material.

### Claim 7 (depends on 4)

The method according to claim 4, wherein the substrate comprises a hardmask comprising an anti-reflective-coating on the substrate between the substrate and the patterned infiltrateable material.

### Claim 8 (depends on 4)

The method according to claim 4, wherein the substrate comprises a hardmask comprising an amorphous carbon film on the substrate between the substrate and the patterned infiltrateable material.

### Claim 9 (depends on 4)

The method according to claim 4, wherein the substrate comprises a hardmask comprising a chemical vapor deposited (CVD) layer between the substrate and the patterned infiltrateable material.

### Claim 10 (depends on 4)

The method according to claim 4, wherein the method comprises while the substrate remains in the sequential infiltration synthesis system removing the infiltrateable material while allowing the infiltration material to remain on the substrate.

### Claim 11 (depends on 10)

The method according to claim 10, wherein removing the infiltrateable material comprises heating the infiltrateable material to a temperature between 80 and 600° C.

### Claim 12 (depends on 10)

The method according to claim 10, wherein removing the infiltrateable material comprises heating the infiltrateable material to a temperature between 100 to 400° C.

### Claim 13 (depends on 10)

The method according to claim 10, wherein removing the infiltrateable material comprises heating the infiltrateable material to a temperature between 120 and 300° C.

### Claim 14 (depends on 10)

The method according to claim 10, wherein the method allows a reduction of the linewidth or the linewidth roughness of the patterned structures of infiltration material with respect to the patterned infiltrateable material.

### Claim 15 (depends on 10)

The method according to claim 10, wherein removing the infiltrateable material comprises providing a plasma to remove the infiltrateable material in the reaction chamber.

### Claim 16 (depends on 4)

The method according to claim 4, wherein the patterned infiltrateable material comprises a patterned photoresist or DSA material.