# US 11,078,595 B2 · Method of producing silicon single crystal ingot and silicon single crystal ingot

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- Number: US 11,078,595 B2
- Document ID: US11078595B2
- Status: Granted
- Kind: B2
- Application number: 16/477,003
- Filed: 2018-01-11
- Published: 2019-11-21
- Granted: 2021-08-03
- Earliest claimed: 2017-02-28
- Assignees: Sumco Corporation
- Applicants: Sumco Corporation
- Inventors: Masataka Hourai; Wataru Sugimura; Toshiaki Ono; Toshiyuki Fujiwara
- Web page: https://patentgrep.com/patent/US11078595B2

## CPC

- C30B 15/20: Controlling or regulating (controlling or regulating in general G05)
- C01B 33/02: Silicon (forming single crystals or homogeneous polycrystalline material with defined structure C30B)
- C30B 29/06: Silicon
- C01P 2002/54: one element only
- C01P 2002/60: Compounds characterised by their crystallite size
- C01P 2006/40: Electric properties
- 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
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Provided is a method of producing a high resistance n-type silicon single crystal ingot with small tolerance margin on resistivity in the crystal growth direction, which is suitably used in a power device. In the method of producing a silicon single crystal ingot using Sb or As as an n-type dopant, while a silicon single crystal ingot is pulled up, the amount of the n-type dopant being evaporated from a silicon melt per unit solidification ratio is kept within a target evaporation amount range per unit solidification ratio by controlling one or more pulling condition values including at least one of the pressure in a chamber, the flow volume of Ar gas, and a gap between a guide portion and the silicon melt.

## Claims

### Claim 1

A method of producing a silicon single crystal ingot using a silicon crystal-pulling furnace having:
a crucible storing a silicon melt doped with an n-type dopant made of Sb or As,
a chamber accommodating the crucible,
a pressure regulator portion controlling a pressure in the chamber,
a pulling portion pulling up a silicon single crystal ingot from the silicon melt,
a gas supply for supplying Ar gas into the chamber, and
a guide portion provided above a surface of the silicon melt for guiding the Ar gas to flow along the surface of the silicon melt, the method comprising:
pulling up the silicon single crystal ingot by the Czochralski process; and
controlling an evaporation amount by keeping an amount of the n-type dopant being evaporated from the silicon melt per unit solidification ratio within a target evaporation amount range per unit solidification ratio by controlling one or more pulling condition values including at least one of a pressure in the chamber, a flow volume of the Ar gas, and a gap between the guide portion and the silicon melt while performing the pulling up the silicon single crystal ingot by the Czochralski process.

### Claim 2 (depends on 1)

The method of producing a silicon single crystal ingot according to claim 1, wherein the target evaporation amount per unit solidification ratio is uniform in a crystal growth direction.

### Claim 3 (depends on 2)

The method of producing a silicon single crystal ingot according to claim 2, further comprising:
prior to the pulling up the silicon single crystal ingot by the Czochralski process:
forming one or more silicon single crystal ingots for evaluation using the silicon single crystal pulling furnace; and
determining changes in the amount of the n-type dopant being evaporated per unit solidification ratio in the silicon single crystal pulling furnace, based on changes in a resistivity of the silicon single crystal ingots for evaporation in a crystal growth direction,
wherein in the controlling the evaporation amount, the pulling condition values are increased or decreased based on the determined changes in the evaporation amount per unit solidification ratio.

### Claim 4 (depends on 2)

The method of producing a silicon single crystal ingot according to claim 2, further comprising measuring the evaporation amount of the n-type dopant per unit solidification ratio while performing the pulling up the silicon single crystal ingot by the Czochralski process
wherein in the controlling the evaporation amount, the pulling condition values are controlled so that the measured evaporation amount per unit solidification ratio is kept within the target evaporation amount per unit solidification ratio.

### Claim 5 (depends on 4)

The method of producing a silicon single crystal ingot according to claim 4, wherein in the measuring the evaporation amount of the n-type dopant per unit solidification ratio, a concentration of the n-type dopant discharged with the Ar gas on an Ar gas outlet side is measured.

### Claim 6 (depends on 5)

The method of producing a silicon single crystal ingot according to claim 5, wherein in the measuring the evaporation amount of the n-type dopant per unit solidification ratio, a diameter and a pulling length of the silicon single crystal ingot being pulled up are measured, and the evaporation amount per unit solidification ratio is calculated on the basis of the solidification ratio based on:
the measurement of the diameter and the pulling length of the silicon single crystal ingot being pulled up, and
the concentration of the n-type dopant contained in the Ar gas.

### Claim 7 (depends on 1)

The method of producing a silicon single crystal ingot according to claim 1, further comprising:
prior to the pulling up the silicon single crystal ingot by the Czochralski process:
forming one or more silicon single crystal ingots for evaluation using the silicon single crystal pulling furnace; and
determining changes in the amount of the n-type dopant being evaporated per unit solidification ratio in the silicon single crystal pulling furnace, based on changes in a resistivity of the silicon single crystal ingots for evaluation in a crystal growth direction,
wherein in the controlling the evaporation amount, the pulling condition values are increased or decreased based on the determined changes in the evaporation amount per unit solidification ratio.

### Claim 8 (depends on 1)

The method of producing a silicon single crystal ingot according to claim 1, further comprising measuring the evaporation amount of the n-type dopant per unit solidification ratio while performing the pulling up the silicon single crystal ingot by the Czochralski process,
wherein in the controlling the evaporation amount, the pulling condition values are controlled so that the measured evaporation amount per unit solidification ratio is kept within the target evaporation amount per unit solidification ratio.

### Claim 9 (depends on 8)

The method of producing a silicon single crystal ingot according to claim 8, wherein in the measuring the evaporation amount of the n-type dopant per unit solidification ratio, a concentration of the n-type dopant discharged with the Ar gas on an Ar gas outlet side is measured.

### Claim 10 (depends on 9)

The method of producing a silicon single crystal ingot according to claim 9, wherein in the measuring the evaporation amount of the n-type dopant per unit solidification ratio, a diameter and a pulling length of the silicon single crystal ingot being pulled up are measured, and the evaporation amount per unit solidification ratio is calculated on the basis of the solidification ratio based on:
the measurement of the diameter and the pulling length of the silicon single crystal ingot being pulled up, and
the concentration of the n-type dopant contained in the Ar gas.