JP6067927B2 - Copper or copper alloy sputtering target - Google Patents

Copper or copper alloy sputtering target Download PDF

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JP6067927B2
JP6067927B2 JP2016511553A JP2016511553A JP6067927B2 JP 6067927 B2 JP6067927 B2 JP 6067927B2 JP 2016511553 A JP2016511553 A JP 2016511553A JP 2016511553 A JP2016511553 A JP 2016511553A JP 6067927 B2 JP6067927 B2 JP 6067927B2
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target
sputtering
ultrasonic flaw
copper
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JPWO2015151901A1 (en
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富男 大月
富男 大月
長田 健一
健一 長田
岡部 岳夫
岳夫 岡部
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JX Nippon Mining and Metals Corp
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • C22C9/01Alloys based on copper with aluminium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • C22C9/05Alloys based on copper with manganese as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/04Analysing solids
    • G01N29/043Analysing solids in the interior, e.g. by shear waves
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/34Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3402Gas-filled discharge tubes operating with cathodic sputtering using supplementary magnetic fields
    • H01J37/3405Magnetron sputtering
    • H01J37/3408Planar magnetron sputtering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/34Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411Constructional aspects of the reactor
    • H01J37/3414Targets
    • H01J37/3426Material
    • H01J37/3429Plural materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/02Indexing codes associated with the analysed material
    • G01N2291/028Material parameters
    • G01N2291/0289Internal structure, e.g. defects, grain size, texture
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/04Wave modes and trajectories
    • G01N2291/044Internal reflections (echoes), e.g. on walls or defects
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/52Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames
    • H01L23/522Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body
    • H01L23/532Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body characterised by the materials
    • H01L23/53204Conductive materials
    • H01L23/53209Conductive materials based on metals, e.g. alloys, metal silicides
    • H01L23/53228Conductive materials based on metals, e.g. alloys, metal silicides the principal metal being copper
    • H01L23/53238Additional layers associated with copper layers, e.g. adhesion, barrier, cladding layers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001Technical content checked by a classifier
    • H01L2924/0002Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Description

本発明は、LSIをはじめとする半導体装置のウエハ内配線部の形成に用いられる銅又は銅合金スパッタリングターゲットに関する。   The present invention relates to a copper or copper alloy sputtering target used for forming an intra-wafer wiring portion of a semiconductor device such as an LSI.

半導体デバイスの配線材料として、銅配線(比抵抗:1.7μΩ・cm程度)が使用されている。銅配線の形成プロセスとして、配線溝にTaやTaNなどの拡散バリア層を形成した後、銅シード層を形成し、その後、銅配線を形成することが行われている。近年、配線の微細化に伴い、薄くなった拡散バリア層のバリア性能低下を解消するためシード層にアルミニウム(Al)、マンガン(Mn)などを添加した銅合金膜や高純度の銅膜を使用することが行われている。  Copper wiring (specific resistance: about 1.7 μΩ · cm) is used as a wiring material for semiconductor devices. As a process for forming a copper wiring, a diffusion barrier layer such as Ta or TaN is formed in a wiring groove, a copper seed layer is formed, and then a copper wiring is formed. In recent years, with the miniaturization of interconnects, copper alloy films and high-purity copper films with aluminum (Al), manganese (Mn), etc. added to the seed layer have been used to eliminate the barrier performance degradation of thin diffusion barrier layers. To be done.

上記の銅合金膜や高純度銅膜は、銅合金又は銅スパッタリングターゲットを用いて成膜される。安定したデバイス性能、製品歩留まりを確保するためには、スパッタリングで形成された膜の均一性や安定した成膜速度が求められている。一般に、これらの膜の均一性や成膜速度の安定性は、スパッタリングターゲット内の組成、密度、組織などのムラ(不均一性)の影響を受ける。したがって、ターゲット内の組成、密度、組織などの均一性を確認し、これを制御することは非常に重要である。   The copper alloy film or the high purity copper film is formed using a copper alloy or a copper sputtering target. In order to ensure stable device performance and product yield, uniformity of a film formed by sputtering and a stable film formation rate are required. In general, the uniformity of these films and the stability of the deposition rate are affected by unevenness (nonuniformity) such as composition, density, and structure in the sputtering target. Therefore, it is very important to confirm and control the uniformity of the composition, density, structure, etc. in the target.

しかしながら従来、スパッタリングターゲット内の組成、密度、組織などの均一性を確認する方法として、ターゲット面内の数箇所、代表的な部分のみについて、それぞれの物性を測定して、評価するのがほとんどであった。そのため、ターゲットの局所的に存在するムラに関しては見落とされる可能性があり、そのような局所的なムラは、膜の均一性を阻害したり、成膜速度を不安定にしたりすることがあった。特に、配線が微細化しつつある最近の状況では、これらは重大な問題としてクローズアップされている。   However, conventionally, as a method for confirming the uniformity of the composition, density, structure, etc. in the sputtering target, the physical properties of only a few representative portions of the target surface are measured and evaluated. there were. Therefore, the local unevenness of the target may be overlooked, and such local unevenness may disturb the uniformity of the film or make the film formation speed unstable. . In particular, in the recent situation where the wiring is becoming finer, these are highlighted as serious problems.

本出願人は以前、スパッタリングターゲット中の酸化物がスパッタ膜に欠陥を引き起こすことから、超音波探傷機によってターゲット中の酸化物介在物を検出して、これを効果的に抑制する技術を提案した(特許文献1)。また、特許文献2には、スパッタリングターゲットにおいて、複数の欠陥のタイプ(ボイド状欠陥、アルミナ介在物など)を識別することができる非破壊評価方法が開示されており、特許文献3には、寸法と位置で分類された欠陥の種類を識別することができる非破壊評価方法が開示されている。   The present applicant has previously proposed a technique for effectively suppressing this by detecting oxide inclusions in the target with an ultrasonic flaw detector because the oxide in the sputtering target causes defects in the sputtered film. (Patent Document 1). Patent Document 2 discloses a nondestructive evaluation method that can identify a plurality of defect types (void-like defects, alumina inclusions, etc.) in a sputtering target. And a non-destructive evaluation method that can identify the types of defects classified by position.

特開2001−011610号公報JP 2001-011610 A 特表2003−532895号公報Special table 2003-532895 gazette 特表2004−538463号公報JP-T-2004-538463

本発明は、半導体装置の配線の形成に適した銅又は銅合金スパッタリングターゲットに関し、特に、スパッタリングターゲット中に局所的に存在する組成、密度、組織などのムラ(不均一性)を制御することができ、これにより、スパッタリング時の成膜速度を安定にすることができると伴に、スパッタ成膜した膜の均一性を向上することができる銅又は銅合金スパッタリグターゲットを提供することを課題とする。  The present invention relates to a copper or copper alloy sputtering target suitable for forming wiring of a semiconductor device, and in particular, to control unevenness (non-uniformity) such as composition, density, and structure present locally in the sputtering target. It is possible to provide a copper or copper alloy sputter target capable of stabilizing the film formation rate during sputtering and improving the uniformity of the film formed by sputtering. To do.

上記の課題を解決するために、本発明者らは、スパッタリングターゲット中に局所的に存在する組成、密度、組織などのムラについて鋭意研究した結果、スパッタリングターゲット全体を超音波探傷機による反射強度で評価し、制御することで、ターゲットの局所的なムラを抑制することができるとの知見を得た。そしてまた、このような局所的なムラの少ないターゲットは、ターゲット製造時の鍛造温度を調整することが特に有効であるとの知見を得た。   In order to solve the above problems, the present inventors have conducted intensive research on unevenness of the composition, density, structure, and the like that are locally present in the sputtering target, and as a result, the entire sputtering target is reflected with an ultrasonic flaw detector. We obtained knowledge that local unevenness of the target can be suppressed by evaluating and controlling. In addition, it has been found that it is particularly effective to adjust the forging temperature at the time of manufacturing the target for such a target with little local unevenness.

これらの知見に基づいて、本発明者らは、以下の発明を提供するものである。
1)ターゲット表面の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定において、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の30%以下であることを特徴とする銅又は銅合金スパッタリングターゲット。
2)ターゲット表面の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定において、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の20%以下であることを特徴とする銅又は銅合金スパッタリングターゲット。
3)ターゲット表面の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定において、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の10%以下であることを特徴とする銅又は銅合金スパッタリングターゲット。
4)Cu、Cu−Al合金、Cu−Mn合金のいずれか一種からなることを特徴とする上記1)〜3)のいずれか一に記載の銅又は銅合金スパッタリングターゲット。
Based on these findings, the present inventors provide the following inventions.
1) In ultrasonic flaw measurement where sensitivity is adjusted so that the intensity of the reflected echo from the bottom of the target when an ultrasonic wave is applied to the reference point is set to 100% as a reference point, A copper or copper alloy sputtering target characterized in that the area of the target detected when the intensity of the reflected echo from the bottom surface is 65% or less or 135% or more is 30% or less of the entire target.
2) In ultrasonic flaw detection with the sensitivity adjusted so that the intensity of the reflected echo from the bottom of the target when an ultrasonic wave is applied to the reference point is set to 100% as a reference point, A copper or copper alloy sputtering target, wherein the target area detected when the intensity of the reflected echo from the bottom surface is 65% or less or 135% or more is 20% or less of the entire target.
3) In ultrasonic flaw detection where sensitivity is adjusted so that the intensity of the reflected echo from the bottom surface of the target when an ultrasonic wave is applied to the reference point is set to 100% as a reference point, A copper or copper alloy sputtering target characterized in that the area of the target detected when the intensity of the reflected echo from the bottom surface is 65% or less or 135% or more is 10% or less of the entire target.
4) The copper or copper alloy sputtering target according to any one of 1) to 3) above, which is made of any one of Cu, Cu—Al alloy, and Cu—Mn alloy.

本発明は、スパッタリングターゲットの組成、密度、組織などのムラ(不均一性)を示す指標として、ターゲットからの超音波の反射強度を用いることで、このようなムラの少ないターゲットを得ることができる。そして、このようなムラの少ないターゲットは膜の均一性を向上することができるとともに、成膜速度を安定化することができるという優れた効果を有する。  The present invention can obtain such a target with little unevenness by using the reflection intensity of ultrasonic waves from the target as an index indicating unevenness (non-uniformity) of the composition, density, structure, etc. of the sputtering target. . Such a target with little unevenness can improve the uniformity of the film and has an excellent effect of stabilizing the film formation rate.

超音波探傷の測定方法を示した説明図である。It is explanatory drawing which showed the measuring method of ultrasonic flaw detection.

本発明の銅又は銅合金スパッタリングターゲットは、ターゲット表面の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定において、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の30%以下であることを特徴とするものである。好ましくは、ターゲットの前記領域が20%以下であり、さらに好ましくは10%以下であることを特徴とするものである。  The copper or copper alloy sputtering target of the present invention uses an arbitrary one point on the target surface as a reference point, and the sensitivity is such that the intensity of the reflected echo from the bottom of the target when an ultrasonic wave is applied to the reference point is 100%. In the adjusted ultrasonic flaw detection measurement, the target area detected when the intensity of the reflected echo from the target bottom surface is 65% or less or 135% or more is 30% or less of the entire target. Preferably, the region of the target is 20% or less, more preferably 10% or less.

超音波探傷機は、探針をスパッタリングターゲット全面に走査させて、ターゲット内の欠陥から反射される波形の強度を調べることで、欠陥のサイズや位置などを把握することができる。欠陥は、ターゲットの組成、密度、組織などのムラ(不均一性)を生じさせることから、このような欠陥を適切に制御することにより、ムラの少ないターゲットを得ることができる。そして、このようなムラの少ないターゲットは、成膜される膜の均一性を向上することができるとともに、スパッタリング時のパーティクル量を低減することができる。  The ultrasonic flaw detector can grasp the size and position of the defect by scanning the entire surface of the sputtering target and examining the intensity of the waveform reflected from the defect in the target. Defects cause unevenness (non-uniformity) in the composition, density, structure, etc. of the target, and thus a target with less unevenness can be obtained by appropriately controlling such defects. Such a target with little unevenness can improve the uniformity of a film to be formed, and can reduce the amount of particles during sputtering.

超音波による探傷は標準試料や設定した基準点での底面からの反射エコーとの比較を行うことにより欠陥や組織等の相違を検出する検査方法であるため、相対評価を行える標準試料又は基準点の設定が必要となる。本発明では、超音波探傷機の感度調整をターゲット表面の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように調整を行う。このようにターゲット底面からの反射エコーをモニターすることにより、材料中の欠陥や組織・組成等の相違を検出することができる。このような感度調整下において、反射エコーの強度が65%以下又は135%以上は、基準となる位置と比較して、材料内に材料欠陥や、組織、組成等の大きな相違があることを意味する。  Ultrasonic flaw detection is an inspection method that detects differences in defects, tissues, etc. by comparing with a standard sample or a reflected echo from the bottom surface at a set reference point. Setting is required. In the present invention, the sensitivity of the ultrasonic flaw detector is adjusted at any one point on the target surface as a reference point, and the intensity of the reflected echo from the target bottom surface when the ultrasonic wave is applied to the reference point is 100%. Make adjustments. By monitoring the reflected echo from the bottom surface of the target in this way, it is possible to detect differences in defects, structures, compositions, etc. in the material. Under such sensitivity adjustment, when the intensity of the reflected echo is 65% or less or 135% or more, it means that there is a large difference in material defects, structure, composition, etc. in the material compared to the reference position. To do.

本発明のスパッタリングターゲットは、銅又は銅合金から構成されるものである。銅としては、純度4N以上のCuを用いることが好ましく、銅合金としては、耐EM性を向上させるために、Alを添加したCu−Al合金、Mnを添加したCu−Mn合金を用いることが好ましい。配線抵抗がデバイスに影響を与えることなく、耐EM性の効果を得るために、特に、Alを0.05〜10wt%添加したCu−Al合金、Mnを0.1〜25wt%添加したCu−Mn合金が好ましい。  The sputtering target of the present invention is composed of copper or a copper alloy. As the copper, it is preferable to use Cu having a purity of 4N or more, and as the copper alloy, in order to improve the EM resistance, it is preferable to use a Cu—Al alloy added with Al or a Cu—Mn alloy added with Mn. preferable. In order to obtain the effect of EM resistance without the wiring resistance affecting the device, in particular, Cu—Al alloy added with 0.05 to 10 wt% Al, Cu—added with 0.1 to 25 wt% Mn A Mn alloy is preferred.

銅又は銅合金スパッタリングターゲットは、原料を溶解及び鋳造し、鋳造後の素材を結晶組織、粒径等を適切なものとするため鍛造や圧延等の塑性加工処理及び熱処理を施し、その後、円板状などの最終ターゲット寸法に仕上げることにより作製される。スパッタリングターゲットにおける超音波探傷による反射強度の制御は、特に鍛造時の温度を各材料にあった適切な温度に調整することが有効であり、本発明の組成にあっては、900℃以下とすることが好ましい。  Copper or copper alloy sputtering target melts and casts the raw material, and performs plastic working and heat treatment such as forging and rolling to make the cast material suitable for crystal structure, grain size, etc. It is produced by finishing to the final target dimension such as a shape. Control of the reflection intensity by ultrasonic flaw detection in the sputtering target is particularly effective to adjust the temperature during forging to an appropriate temperature suitable for each material. In the composition of the present invention, the temperature is set to 900 ° C. or lower. It is preferable.

次に、実施例に基づいて本発明を説明する。以下に示す実施例は、理解を容易にするためのものであり、これらの実施例によって本発明を制限するものではない。すなわち、本発明の技術思想に基づく変形及び他の実施例は、当然本発明に含まれる。   Next, the present invention will be described based on examples. The following examples are for ease of understanding, and the present invention is not limited by these examples. That is, modifications and other embodiments based on the technical idea of the present invention are naturally included in the present invention.

(実施例1)
純度6N以上の高純度Cuを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、溶湯を鋳型(モールド)に出湯し、純度6N以上の高純度銅インゴットを得た。次に、得られたインゴットを直径180mm×厚さ160mmとした後、420℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、400℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
Example 1
High purity Cu having a purity of 6N or more was prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten metal was poured out into a mold to obtain a high purity copper ingot having a purity of 6N or higher. Next, after making the obtained ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 420 ° C. and further rolled by cold rolling until the reduction ratio reached 70% or more. Then, after heat-processing at 400 degreeC, it rapidly cooled and produced the rolled sheet. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。具体的には、測定対象物であるスパッタリングターゲットを水中に沈めて、探針を対象物全体に走査させ、対象物内の欠陥から反射される波形の強度とその強度の高い領域を算出した。超音波探傷の条件は、以下の通りである。
装置:Krautkramer社製 形式:HIS3
IF音速 :1480m/s
材料音速 :2000〜6000m/s
AMP :≧30dB
感度調整 :円盤状ターゲットの中心を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように調整
その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の5%であった。
The target thus produced was analyzed using an ultrasonic flaw detector. Specifically, the sputtering target as the measurement object was submerged in water, the probe was scanned over the entire object, and the intensity of the waveform reflected from the defect in the object and the region with the high intensity were calculated. The conditions for ultrasonic flaw detection are as follows.
Device: Krautkramer Type: HIS3
IF sound speed: 1480 m / s
Material sound velocity: 2000-6000 m / s
AMP: ≧ 30 dB
Sensitivity adjustment: The center of the disk-shaped target is used as a reference point, and the intensity of the reflected echo from the bottom of the target when ultrasonic waves are applied to the reference point is adjusted to 100%. As a result, the reflection intensity by the ultrasonic flaw detector The target area detected at 35% or more was 5% of the entire target.

次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、投入電力:38kWにてスパッタリングを実施して、12インチのシリコン基板上に5秒間成膜した。そして、スパッタリングで形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。具体的には、ウエハ上の49点のシート抵抗を測定し、その標準偏差(ユニフォーミティ)とユニフォーミティ(NU%)を求めた。標準偏差とユニフォーミティの算出方法は、以下の通りである。
標準偏差(σ)=(((Rs1-RsAve)2+(Rs2-RsAve)2+・・・+(Rs49-RsAve)2)/49)1/2
(Rsn :各測定点でのシート抵抗(Rs)、RsAve: Rsの49点平均値)
ユニフォーミティ(NU%)=σ/ RsAve×100
その結果、標準偏差は0.025であり、ユニフォーミティは3.2%であり、均一性に優れた膜が得られた。以上の結果を表1に示す。
Next, after the target subjected to ultrasonic flaw detection was bonded to a backing plate, it was placed in a sputtering apparatus, and sputtering was performed at an input power of 38 kW to form a film on a 12-inch silicon substrate for 5 seconds. And distribution of the sheet resistance of the film | membrane formed by sputtering was measured, and the distribution condition of film thickness was investigated. Specifically, the sheet resistance at 49 points on the wafer was measured, and the standard deviation (uniformity) and uniformity (NU%) were obtained. The standard deviation and uniformity are calculated as follows.
Standard deviation (σ) = (((Rs 1 -Rs Ave ) 2 + (Rs 2 -Rs Ave ) 2 + ... + (Rs 49 -Rs Ave ) 2 ) / 49) 1/2
(Rsn: sheet resistance (Rs) at each measurement point, RsAve: average value of 49 Rs points)
Uniformity (NU%) = σ / Rs Ave × 100
As a result, the standard deviation was 0.025, the uniformity was 3.2%, and a film having excellent uniformity was obtained. The results are shown in Table 1.

(実施例2)
純度6N以上の高純度Cuを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、溶湯を鋳型(モールド)に出湯し、純度6N以上の高純度銅インゴットを得た。次に、得られたインゴットを直径180mm×厚さ160mmとした後、630℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、400℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Example 2)
High purity Cu having a purity of 6N or more was prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten metal was poured out into a mold to obtain a high purity copper ingot having a purity of 6N or higher. Next, after making the obtained ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 630 ° C., and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 400 degreeC, it rapidly cooled and produced the rolled sheet. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の15%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.036、ユニフォーミティは3.8%であり、均一性に優れた膜が得られた。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected by the ultrasonic flaw detector with a reflection intensity of 35% or more was 15% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.036, the uniformity was 3.8%, and a film having excellent uniformity was obtained. The results are shown in Table 1.

(実施例3)
純度6N以上の高純度Cu、純度3N以上の高純度Mnを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuMn合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Mn合金インゴット(Mn:0.1wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、820℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Example 3)
High-purity Cu having a purity of 6N or higher and high-purity Mn having a purity of 3N or higher were prepared and introduced into a crucible and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuMn alloy was poured into a mold to obtain a high purity Cu—Mn alloy ingot (Mn: 0.1 wt%) having a purity of 5N or more. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 820 ° C. and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の8%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施し、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.027、ユニフォーミティは2.7%であり、均一性に優れた膜が得られた。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected by the ultrasonic flaw detector at a reflection intensity of 35% or more was 8% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.027, the uniformity was 2.7%, and a film having excellent uniformity was obtained. The results are shown in Table 1.

(実施例4)
純度6N以上の高純度Cu、純度4N以上の高純度Mnを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuMn合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Mn合金インゴット(Mn:25wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、780℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
Example 4
High-purity Cu having a purity of 6N or higher and high-purity Mn having a purity of 4N or higher were prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuMn alloy was poured into a mold to obtain a high-purity Cu—Mn alloy ingot (Mn: 25 wt%) having a purity of 5N or more. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 780 ° C., and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.026、ユニフォーミティは3.0%であり、均一性に優れた膜が得られた。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.026, the uniformity was 3.0%, and a film having excellent uniformity was obtained. The results are shown in Table 1.

(実施例5)
純度6N以上の高純度Cu、純度4N以上の高純度Alを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuAl合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Al合金インゴット(Al:0.01wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、820℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Example 5)
High purity Cu having a purity of 6N or higher and high purity Al having a purity of 4N or higher were prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuAl alloy was poured into a mold to obtain a high purity Cu—Al alloy ingot (Al: 0.01 wt%) having a purity of 5N or higher. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 820 ° C. and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.029、ユニフォーミティは3.3%であり、均一性に優れた膜が得られた。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.029, the uniformity was 3.3%, and a film having excellent uniformity was obtained. The results are shown in Table 1.

(実施例6)
純度6N以上の高純度Cu、純度4N以上の高純度Alを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuAl合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Al合金インゴット(Al:10wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、780℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Example 6)
High purity Cu having a purity of 6N or higher and high purity Al having a purity of 4N or higher were prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuAl alloy was poured out into a mold (mold) to obtain a high purity Cu—Al alloy ingot (Al: 10 wt%) having a purity of 5N or more. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 780 ° C., and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.033、ユニフォーミティは3.5%であり、均一性に優れた膜が得られた。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.033, the uniformity was 3.5%, and a film having excellent uniformity was obtained. The results are shown in Table 1.

(比較例1)
純度6N以上の高純度Cuを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、溶湯を鋳型(モールド)に出湯し、純度6N以上の高純度銅インゴットを得た。次に、得られたインゴットを直径180mm×厚さ160mmとした後、950℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、400℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Comparative Example 1)
High purity Cu having a purity of 6N or more was prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten metal was poured out into a mold to obtain a high purity copper ingot having a purity of 6N or higher. Next, after making the obtained ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 950 ° C. and further rolled by cold rolling until the reduction ratio reached 70% or more. Then, after heat-processing at 400 degreeC, it rapidly cooled and produced the rolled sheet. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.051、ユニフォーミティは4.5%であり、実施例に比べて均一性に劣る膜となった。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.051 and the uniformity was 4.5%, and the film was inferior in uniformity compared to the examples. The results are shown in Table 1.

(比較例2)
純度6N以上の高純度Cuを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、溶湯を鋳型(モールド)に出湯し、純度6N以上の高純度銅インゴットを得た。次に、得られたインゴットを直径180mm×厚さ160mmとした後、1000℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、400℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Comparative Example 2)
High purity Cu having a purity of 6N or more was prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten metal was poured out into a mold to obtain a high purity copper ingot having a purity of 6N or higher. Next, after making the obtained ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 1000 ° C., and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 400 degreeC, it rapidly cooled and produced the rolled sheet. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.102、ユニフォーミティは5.1%であり、実施例に比べて均一性に劣る膜となった。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.102 and the uniformity was 5.1%, and the film was inferior in uniformity compared to the examples. The results are shown in Table 1.

(比較例3)
純度6N以上の高純度Cu、純度3N以上の高純度Mnを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuMn合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Mn合金インゴット(Mn:0.1wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、1000℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Comparative Example 3)
High-purity Cu having a purity of 6N or higher and high-purity Mn having a purity of 3N or higher were prepared and introduced into a crucible and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuMn alloy was poured into a mold to obtain a high purity Cu—Mn alloy ingot (Mn: 0.1 wt%) having a purity of 5N or more. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 1000 ° C. and further rolled by cold rolling until the reduction ratio reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.073、ユニフォーミティは4.6%であり、実施例に比べて均一性に劣る膜となった。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus and sputtered under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.073 and the uniformity was 4.6%, and the film was inferior in uniformity compared to the examples. The results are shown in Table 1.

(比較例4)
純度6N以上の高純度Cu、純度4N以上の高純度Mnを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuMn合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Mn合金インゴット(Mn:25wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、980℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Comparative Example 4)
High-purity Cu having a purity of 6N or higher and high-purity Mn having a purity of 4N or higher were prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuMn alloy was poured into a mold to obtain a high-purity Cu—Mn alloy ingot (Mn: 25 wt%) having a purity of 5N or more. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 980 ° C., and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was machined into a disk having a diameter of 450 mm and a thickness of 10 mm, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to produce a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.084、ユニフォーミティは5.2%であり、実施例に比べて均一性に劣る膜となった。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.084, the uniformity was 5.2%, and the film was inferior in uniformity compared to the examples. The results are shown in Table 1.

(比較例5)
純度6N以上の高純度Cu、純度4N以上の高純度Alを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuAl合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Al合金インゴット(Al:0.01wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、1000℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Comparative Example 5)
High purity Cu having a purity of 6N or higher and high purity Al having a purity of 4N or higher were prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuAl alloy was poured into a mold to obtain a high purity Cu—Al alloy ingot (Al: 0.01 wt%) having a purity of 5N or higher. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 1000 ° C. and further rolled by cold rolling until the reduction ratio reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was machined into a disk having a diameter of 450 mm and a thickness of 10 mm, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to produce a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施して、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.093、ユニフォーミティは5.6%であり、実施例に比べて均一性に劣る膜となった。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.093, the uniformity was 5.6%, and the film was inferior in uniformity compared to the examples. The results are shown in Table 1.

(比較例6)
純度6N以上の高純度Cu、純度4N以上の高純度Alを用意し、これを坩堝に導入して、1250℃で溶解した(誘導溶解法)。その後、CuAl合金の溶湯を鋳型(モールド)に出湯し、純度5N以上の高純度Cu−Al合金インゴット(Al:10wt%)を得た。次に、得られた銅合金インゴットを直径180mm×厚さ160mmとした後、980℃で熱間鍛造し、さらに冷間圧延で圧下率が70%以上となるまで圧延した。その後、600℃で熱処理した後、急冷して圧延板を作製した。これを機械加工により、直径450mm、厚さ10mmの円板に加工した後、表面粗さが0.8μm以下となるようにペーパー仕上げを行って、ターゲットを作製した。
(Comparative Example 6)
High purity Cu having a purity of 6N or higher and high purity Al having a purity of 4N or higher were prepared, introduced into a crucible, and melted at 1250 ° C. (induction melting method). Thereafter, the molten CuAl alloy was poured out into a mold (mold) to obtain a high purity Cu—Al alloy ingot (Al: 10 wt%) having a purity of 5N or more. Next, after making the obtained copper alloy ingot 180 mm in diameter × 160 mm in thickness, it was hot forged at 980 ° C., and further rolled by cold rolling until the reduction rate reached 70% or more. Then, after heat-processing at 600 degreeC, it cooled rapidly and the rolled sheet was produced. This was processed into a disk having a diameter of 450 mm and a thickness of 10 mm by machining, and then paper finishing was performed so that the surface roughness was 0.8 μm or less to prepare a target.

このようにして作製したターゲットについて、超音波探傷機を用いて分析を行った。超音波探傷の条件は、実施例1と同様にした。その結果、超音波探傷機による反射強度35%以上で検出されるターゲットの領域がターゲット全体の13%であった。次に、超音波探傷を行ったターゲットをバッキングプレートに接合後、スパッタ装置に設置し、実施例1と同様の条件でスパッタリングを実施し、成膜した。そして、実施例1と同様に形成した膜のシート抵抗の分布を測定して、膜厚の分布状況を調べた。その結果、標準偏差は0.110、ユニフォーミティは6.7%であり、実施例に比べて均一性に劣る膜となった。以上の結果を表1に示す。  The target thus produced was analyzed using an ultrasonic flaw detector. The conditions for ultrasonic flaw detection were the same as in Example 1. As a result, the target area detected with an ultrasonic flaw detector having a reflection intensity of 35% or more was 13% of the entire target. Next, after the target subjected to ultrasonic flaw detection was bonded to the backing plate, it was placed in a sputtering apparatus, and sputtering was performed under the same conditions as in Example 1 to form a film. And the distribution of the sheet resistance of the film | membrane formed similarly to Example 1 was measured, and the distribution condition of the film thickness was investigated. As a result, the standard deviation was 0.110, and the uniformity was 6.7%, and the film was inferior in uniformity compared to the examples. The results are shown in Table 1.

本発明は、銅又は銅合金スパッタリングターゲットにおいて、均一性に優れたスパッタ成膜特性を有し、安定した成膜速度を維持することができるので、半導体装置の配線層、特にシード層を安定的に形成するのに有用である。  The present invention has a sputter deposition characteristic with excellent uniformity in a copper or copper alloy sputtering target, and can maintain a stable deposition rate, so that a wiring layer of a semiconductor device, particularly a seed layer can be stably formed. Useful to form.

Claims (4)

ターゲット面内の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定によってターゲット面全体を測定し、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の30%以下であるターゲットをスパッタリングターゲットとして選択し、前記スパッタリングターゲットをスパッタリングして銅又は銅合金配線形成することを特徴とするスパッタリング成膜方法Any one position in the target plane as a reference point, thus the target surface to the ultrasonic flaw detection measurements sensitivity adjustment so that the intensity of the reflected echo becomes 100% from the target bottom surface when irradiated with ultrasonic wave to the reference point The entire target is measured, and a target whose target area detected when the intensity of the reflected echo from the target bottom surface is 65% or less or 135% or more is 30% or less of the entire target surface is selected as the sputtering target, sputtering deposition method and forming a sputtering to copper or a copper alloy wiring. ターゲット面内の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定によってターゲット面全体を測定し、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の20%以下であるターゲットをスパッタリングターゲットとして選択し、前記スパッタリングターゲットをスパッタリングして銅又は銅合金配線形成することを特徴とするスパッタリング成膜方法Any one position in the target plane as a reference point, thus the target surface to the ultrasonic flaw detection measurements sensitivity adjustment so that the intensity of the reflected echo becomes 100% from the target bottom surface when irradiated with ultrasonic wave to the reference point The entire target is measured, and a target whose target area detected when the intensity of the reflected echo from the target bottom surface is 65% or less or 135% or more is 20% or less of the entire target surface is selected as the sputtering target. sputtering deposition method and forming a sputtering to copper or a copper alloy wiring. ターゲット面内の任意の1箇所を基準点とし、その基準点に超音波を当てたときのターゲット底面からの反射エコーの強度を100%となるように感度調整した超音波探傷測定によってターゲット面全体を測定し、ターゲット底面からの反射エコーの強度が65%以下又は135%以上で検出されるターゲットの領域がターゲット全体の10%以下であるターゲットをスパッタリングターゲットとして選択し、前記スパッタリングターゲットをスパッタリングして銅又は銅合金配線形成することを特徴とするスパッタリング成膜方法Any one position in the target plane as a reference point, thus the target surface to the ultrasonic flaw detection measurements sensitivity adjustment so that the intensity of the reflected echo becomes 100% from the target bottom surface when irradiated with ultrasonic wave to the reference point The entire target is measured, and a target whose target area detected when the intensity of reflected echo from the target bottom surface is 65% or less or 135% or more is 10% or less of the entire target surface is selected as the sputtering target, sputtering deposition method and forming a sputtering to copper or a copper alloy wiring. 前記ターゲットが、Cu、Cu−Al合金、Cu−Mn合金のいずれか一種からなることを特徴とする請求項1〜3のいずれか一項に記載の成膜方法The film formation method according to claim 1 , wherein the target is made of any one of Cu, Cu—Al alloy, and Cu—Mn alloy.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210005328A (en) * 2017-03-30 2021-01-13 제이엑스금속주식회사 Sputtering target and manufacturing method therefor
KR102362400B1 (en) * 2017-03-30 2022-02-14 제이엑스금속주식회사 Sputtering target and manufacturing method therefor

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