# US 10,770,274 B2 · Copper alloy sputtering target and manufacturing method of copper alloy sputtering target

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- Number: US 10,770,274 B2
- Document ID: US10770274B2
- Status: Granted
- Kind: B2
- Application number: 15/480,733
- Filed: 2017-04-06
- Published: 2017-07-27
- Granted: 2020-09-08
- Earliest claimed: 2013-07-31
- Assignees: Mitsubishi Materials Corporation
- Applicants: Mitsubishi Materials Corporation
- Inventors: Satoru Mori; Toshio Sakamoto; Kiyoyuki Ookubo
- Web page: https://patentgrep.com/patent/US10770274B2

## CPC

- H01J 37/3429: {Plural materials}
- B22D 7/005: {from non-ferrous metals}
- B22D 11/004: {Copper alloys}
- B22D 11/108: Feeding additives, powders, or the like
- C22C 1/02: by melting {(C22C1/1036 takes precedence)}
- C22C 9/00: Alloys based on copper
- C22F 1/08: of copper or alloys based thereon
- C23C 14/3414: {Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy}
- H01J 37/3491: {Manufacturing of targets}
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- B22D: CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES (shaping of plastics or substances in a plastic state B29C; metallurgical processing, selection of substances to be added to metal C21, C22)
- C22C: ALLOYS (treatment of alloys C21D, C22F)
- C22F: CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS (surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by this subclass, C23F17/00)
- 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)

## Abstract

A copper alloy sputtering target is formed by a copper alloy including the content of Ca being 0.3 to 1.7% by mass, the total content of Mg and Al being 5 ppm or less by mass, the content of oxygen being 20 ppm or less by mass, and the remainder is Cu and inevitable impurities. A manufacturing method of a copper alloy sputtering target comprises steps of: preparing a copper having purity of 99.99% or more by mass; melting the copper so as to obtain a molten copper; controlling components so as to obtain a molten metal having a predetermined component composition by the addition of Ca having a purity of 98.5% or more by mass into the molten copper and by melting the Ca; casting the molten metal so as to obtain an ingot; and performing stress relieving annealing after performing hot rolling to the ingot.

## Claims

### Claim 1

A manufacturing method of a copper alloy sputtering target, the sputtering target formed by a copper alloy containing: the content of Ca being 0.3 to 1.7% by mass; the total content of Mg and Al being 5 ppm or less by mass; the content of oxygen being 20 ppm or less by mass; and the remainder is Cu and inevitable impurities, the manufacturing method comprising the steps of:
preparing a copper having purity of 99.99% or more by mass;
melting the copper by a high frequency induction heating in a crucible in an inert gas atmosphere or a reducing gas atmosphere so as to obtain a molten copper;
controlling component so as to obtain a molten metal having a predetermined component compositions by the addition of Ca having purity of 98.5% or more by mass into the molten copper and by melting the Ca;
casting the molten metal having the predetermined component compositions in a cooled casting mold so as to obtain an ingot; and
performing stress relieving annealing after performing hot-rolling to the ingot,
and wherein the copper alloy sputtering target causes no abnormal discharge when sputtering for 8 hours at an output of 600 W by using direct current system as a power supply,
wherein the abnormal discharge is counted using an arc counter provided in the power supply, and
wherein the sputtering is performed under conditions of evacuating a vacuum chamber of a sputtering apparatus to a vacuum pressure of 4×10−5 Pa or less, and then supplying an oxygen-Ar mixed gas including pure Ar gas or oxygen in a proportion of 10% by volume into the vacuum chamber as a sputtering gas to set a pressure of a sputtering atmosphere to 0.67 Pa.

### Claim 2 (depends on 1)

The manufacturing method of the copper alloy sputtering target according to claim 1, wherein
in the step of the controlling the components, additive materials for the Ca are used by selecting Ca additives in which the content of Mg and Al is 50 ppm or less by mass respectively and the total content of Mg and Al is 100 ppm or less by mass.

### Claim 3 (depends on 1)

The manufacturing method of the copper alloy sputtering target according to claim 1, wherein
the casting method in the casting so as to obtain the ingot is a semi-continuous casting method in which melting materials are melted using a batch furnace and casting only is continuously performed in a predetermined length or a fully-continuous casting method in which melting materials are continuously melted and casting is continuously performed in length unlimited in principle.

### Claim 4

A manufacturing method of a copper alloy sputtering target, the sputtering target formed by a copper alloy containing: the content of Ca being 0.3 to 1.7% by mass; the total content of Mg and Al being 5 ppm or less by mass; the content of oxygen being 20 ppm or less by mass; and the remainder is Cu and inevitable impurities, with Fe, Mn and Si being contained as the inevitable impurities in the copper alloy sputtering target, and the content of Fe is 1 ppm or less by mass, the content of Mn is 1 ppm or less by mass, and the content of Si is 1 ppm or less by mass, the manufacturing method comprising the steps of:
preparing a copper having purity of 99.99% or more by mass;
melting the copper by a high frequency induction heating in a crucible in an inert gas atmosphere or a reducing gas atmosphere so as to obtain a molten copper;
controlling component so as to obtain a molten metal having a predetermined component compositions by the addition of Ca having purity of 98.5% or more by mass into the molten copper and by melting the Ca;
casting the molten metal having the predetermined component compositions in a cooled casting mold so as to obtain an ingot; and
performing stress relieving annealing after performing hot-rolling to the ingot,
and wherein the copper alloy sputtering target causes no abnormal discharge when sputtering for 8 hours at an output of 600 W by using direct current system as a power supply,
wherein the abnormal discharge is counted using an arc counter provided in the power supply, and
wherein the sputtering is performed under conditions of evacuating a vacuum chamber of a sputtering apparatus to a vacuum pressure of 4×10−5 Pa or less, and then supplying an oxygen-Ar mixed gas including pure Ar gas or oxygen in a proportion of 10% by volume into the vacuum chamber as a sputtering gas to set a pressure of a sputtering atmosphere to 0.67 Pa.

### Claim 5 (depends on 4)

The manufacturing method of the copper alloy sputtering target according to claim 4, wherein in the step of the controlling the components, additive materials for the Ca are used by selecting Ca additives in which the content of Mg and Al is 50 ppm or less by mass respectively and the total content of Mg and Al is 100 ppm or less by mass.

### Claim 6 (depends on 2)

The manufacturing method of the copper alloy sputtering target according to claim 2, wherein the casting method in the casting so as to obtain the ingot is a semi-continuous casting method in which melting materials are melted using a batch furnace and casting only is continuously performed in a predetermined length or a fully-continuous casting method in which melting materials are continuously melted and casting is continuously performed in length unlimited in principle.

### Claim 7 (depends on 4)

The manufacturing method of the copper alloy sputtering target according to claim 4, wherein the casting method in the casting so as to obtain the ingot is a semi-continuous casting method in which melting materials are melted using a batch furnace and casting only is continuously performed in a predetermined length or a fully-continuous casting method in which melting materials are continuously melted and casting is continuously performed in length unlimited in principle.

### Claim 8 (depends on 5)

The manufacturing method of the copper alloy sputtering target according to claim 5, wherein the casting method in the casting so as to obtain the ingot is a semi-continuous casting method in which melting materials are melted using a batch furnace and casting only is continuously performed in a predetermined length or a fully-continuous casting method in which melting materials are continuously melted and casting is continuously performed in length unlimited in principle.

### Claim 9

A manufacturing method of a copper alloy sputtering target, the sputtering target being the copper alloy sputtering target, the manufacturing method comprising the steps of:
preparing a copper having purity of 99.99% or more by mass;
melting the copper by a high frequency induction heating in a crucible in an inert gas atmosphere or a reducing gas atmosphere so as to obtain a molten copper;
controlling component so as to obtain a molten metal having a predetermined component compositions by the addition of Ca having purity of 98.5% or more by mass into the molten copper and by melting the Ca;
casting the molten metal having the predetermined component compositions in a cooled casting mold so as to obtain an ingot; and
performing stress relieving annealing after performing hot-rolling to the ingot,
and wherein the copper alloy sputtering target causes no abnormal discharge when sputtering for 8 hours at an output of 600 W by using direct current system as a power supply,
wherein the abnormal discharge is counted using an arc counter provided in the power supply, and
wherein the sputtering is performed under conditions of evacuating a vacuum chamber of a sputtering apparatus to a vacuum pressure of 4×10−5 Pa or less, and then supplying an oxygen-Ar mixed gas including pure Ar gas or oxygen in a proportion of 10% by volume into the vacuum chamber as a sputtering gas to set a pressure of a sputtering atmosphere to 0.67 Pa.

### Claim 10 (depends on 1)

The manufacturing method of the copper alloy sputtering target according to claim 1, wherein
the copper is an oxygen-free copper containing a content of Al, Si, Mg, and Fe of 1 ppm or less by mass for each.

### Claim 11 (depends on 4)

The manufacturing method of the copper alloy sputtering target according to claim 4, wherein
the copper is an oxygen-free copper containing a content of Al, Si, Mg, and Fe of 1 ppm or less by mass for each.

### Claim 12 (depends on 9)

The manufacturing method of the copper alloy sputtering target according to claim 9, wherein
the copper is an oxygen-free copper containing a content of Al, Si, Mg, and Fe of 1 ppm or less by mass for each.