# US 12,180,611 B2 · Methods of forming silicon carbide coated base substrates at multiple temperatures

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- Number: US 12,180,611 B2
- Document ID: US12180611B2
- Status: Granted
- Kind: B2
- Application number: 18/492,482
- Filed: 2023-10-23
- Published: 2024-02-15
- Granted: 2024-12-31
- Earliest claimed: 2021-01-12
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Yen Lin Leow; Xinning Luan; Hui Chen; Kirk Allen Fisher; Shawn Thomas
- Web page: https://patentgrep.com/patent/US12180611B2

## CPC

- C30B 25/16: Controlling or regulating (controlling or regulating in general G05)
- C30B 25/10: Heating of the reaction chamber or the substrate
- C30B 25/18: characterised by the substrate
- C30B 29/36: Carbides
- C30B 29/68: Crystals with laminate structure, e.g. "superlattices"
- 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

Embodiments of the present disclosure generally relate to silicon carbide coated base substrates, silicon carbide substrates thereof, and methods for forming silicon carbide coated base substrates. In some embodiments, a method includes introducing a first silicon-containing precursor to a process chamber at a first temperature of about 800° C. to less than 1,000° C. to form a first silicon carbide layer on a base substrate. The method includes introducing a second silicon-containing precursor, that is the same or different than the first silicon-containing precursor, to the process chamber at a second temperature of about 1,000° C. to about 1,400° C. to form a second silicon carbide layer on the first silicon carbide layer.

## Claims

### Claim 1

A method, comprising:
flowing a first silicon-containing precursor to a process chamber at a first temperature of 1,000° C. to 1,400° C.;
during flowing of the first silicon-containing precursor, decreasing the first temperature to a second temperature of 800° C. to less than 1,000° C. to form a first silicon carbide layer on a base substrate; and
flowing a second silicon-containing precursor, that is the same as or different than the first silicon-containing precursor, to the process chamber at a third temperature, that is the same as or different than the first temperature, of 1,000° C. to 1,400° C. to form a second silicon carbide layer on the first silicon carbide layer.

### Claim 2 (depends on 1)

The method of claim 1, wherein the base substrate is a graphite.

### Claim 3 (depends on 1)

The method of claim 1, wherein:
the first silicon-containing precursor is dimethyldichlorosilane, and
the method further comprises flowing hydrogen to the process chamber substantially concurrently with the first silicon-containing precursor.

### Claim 4 (depends on 1)

The method of claim 1, further comprising removing the first silicon carbide layer and the second silicon carbide layer from the base substrate to form a silicon carbide substrate, wherein the silicon carbide substrate has a degree of warpage or bow of 50 microns to 1 millimeter, as determined by ASTM F534.

### Claim 5 (depends on 1)

The method of claim 1, wherein:
the first temperature is 1,125° C. to 1,300° C.;
the second temperature is 850° C. to 950° C.; and
the third temperature is 1,125° C. to 1,300° C.

### Claim 6 (depends on 4)

The method of claim 4, wherein the first silicon carbide layer has:
a first side proximate the base substrate, the first side having an Si content of 50 mol % to 100 mol % (as determined at a depth of the first side of 0 micron to 1 micron), and
a second side proximate the second silicon carbide layer, the second side having a carbon content of 50 mol % to 100 mol % (as determined at a depth of the second side of 0 micron to 1 micron).

### Claim 7 (depends on 1)

The method of claim 1, wherein the first silicon carbide layer has a carbon content of 50 mol % to 100 mol %.

### Claim 8 (depends on 1)

The method of claim 1, wherein the first silicon carbide layer has a density of 2.3 g/cm3 to 3.21 g/cm3, as determined by ASTM C 559.

### Claim 9 (depends on 1)

The method of claim 1, wherein:
the first silicon carbide layer has a coefficient of thermal expansion between of 3×10E−6/° C. to 5×10E−6/° C., as determined by ASTM E228-17;
the second silicon carbide layer has a coefficient of thermal expansion (CTE) of 1×10E−6/° C. to 4×10E−6/° C., as determined by ASTM E228-17; and
the base substrate has a coefficient of thermal expansion of 4×10E−6/° C. to 8×10E−6/° C., as determined by ASTM E228-17.

### Claim 10 (depends on 1)

The method of claim 1, wherein:
the first silicon carbide layer has a lattice constant (a (Å)) of 4 Å to 7 Å, as determined by ASTM E1426-14 and a lattice constant (c (Å)) of 4 Å to 7 Å, as determined by ASTM E1426-14;
the second silicon carbide layer has a lattice constant (a (Å)) of 3 Å to 6 Å, as determined by ASTM E1426-14, and a lattice constant (c (Å)) of 3 Å to 6 Å, as determined by ASTM E1426-14; and
the base substrate has a lattice constant (a (Å)) of 1 Å to 4 Å, as determined by ASTM E1426-14, and a lattice constant (c (Å)) of 5 Å to 8 Å, as determined by ASTM E1426-14.

### Claim 11 (depends on 1)

The method of claim 1, wherein:
the first silicon carbide layer has a thickness of 1 micron to less than 200 microns; and
the second silicon carbide layer has a thickness of 40 microns to 1.5 millimeters.

### Claim 12

A method, comprising:
flowing a first silicon-containing precursor to a process chamber at a first temperature of 1,000° C. to 1,400° C.;
during flowing of the first silicon-containing precursor, decreasing the first temperature to a second temperature of 800° C. to less than 1,000° C. to form an amorphous first silicon carbide layer on a base substrate; and
flowing a second silicon-containing precursor, that is the same as or different than the first silicon-containing precursor, to the process chamber at a third temperature, that is the same as or different than the first temperature, of 1,000° C. to 1,400° C. to form a polycrystalline second silicon carbide layer on the amorphous first silicon carbide layer.

### Claim 13 (depends on 12)

The method of claim 12, wherein the base substrate is a graphite.

### Claim 14 (depends on 12)

The method of claim 12, wherein:
the first silicon-containing precursor is SiH4; and
the method further comprises flowing a hydrocarbon to the process chamber substantially concurrently with the first silicon-containing precursor.

### Claim 15 (depends on 12)

The method of claim 12, further comprising removing the amorphous first silicon carbide layer and the polycrystalline second silicon carbide layer from the base substrate to form a silicon carbide substrate, wherein the silicon carbide substrate has a degree of warpage or bow of 50 microns to 1 millimeter, as determined by ASTM F534.

### Claim 16 (depends on 13)

The method of claim 13 wherein the graphite has a pore size of 0.4 to 5 μm and a degree of porosity of 6% to 15%.

### Claim 17

A method, comprising:
flowing a first silicon-containing precursor to a process chamber at a first temperature;
during flowing of the first silicon-containing precursor, decreasing the first temperature to a second temperature to form an amorphous first silicon carbide layer on a base substrate; and
flowing a second silicon-containing precursor, that is the same as or different than the first silicon-containing precursor, to the process chamber at a third temperature, that is the same as or different than the first temperature, to form a polycrystalline second silicon carbide layer on the amorphous first silicon carbide layer.

### Claim 18 (depends on 17)

The method of claim 17, wherein:
the first silicon-containing precursor is flowed at a first flow rate of 2 standard liters per minute (slpm) to 200 slpm; and
the second silicon-containing precursor is flowed at a second flow rate of 2 slpm to 200 slpm.

### Claim 19 (depends on 17)

The method of claim 17, further comprising:
decreasing the third temperature to a fourth temperature; and
removing the amorphous first silicon carbide layer and the polycrystalline second silicon carbide layer from the base substrate to form a silicon carbide substrate using an O2 ashing process.

### Claim 20 (depends on 18)

The method of claim 18, further comprising removing the amorphous first silicon carbide layer from the polycrystalline second silicon carbide layer using an O2 ashing process.