JP4476827B2 - Method for producing sputtering target material - Google Patents
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- JP4476827B2 JP4476827B2 JP2005020951A JP2005020951A JP4476827B2 JP 4476827 B2 JP4476827 B2 JP 4476827B2 JP 2005020951 A JP2005020951 A JP 2005020951A JP 2005020951 A JP2005020951 A JP 2005020951A JP 4476827 B2 JP4476827 B2 JP 4476827B2
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- 239000013077 target material Substances 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000005477 sputtering target Methods 0.000 title claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 40
- 239000002184 metal Substances 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 36
- 229910045601 alloy Inorganic materials 0.000 claims description 25
- 239000000956 alloy Substances 0.000 claims description 25
- 238000010587 phase diagram Methods 0.000 claims description 15
- 239000006104 solid solution Substances 0.000 claims description 14
- 238000007731 hot pressing Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229910002056 binary alloy Inorganic materials 0.000 claims description 7
- 229910000765 intermetallic Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 description 23
- 239000000203 mixture Substances 0.000 description 16
- 238000000465 moulding Methods 0.000 description 10
- 238000001513 hot isostatic pressing Methods 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 238000005204 segregation Methods 0.000 description 5
- 229910021332 silicide Inorganic materials 0.000 description 5
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001192 hot extrusion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910019819 Cr—Si Inorganic materials 0.000 description 1
- 229910017060 Fe Cr Inorganic materials 0.000 description 1
- 229910002544 Fe-Cr Inorganic materials 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Description
本発明は、高強度、均質な性能を持つスパッタリングターゲット材の製造方法に関するものである。 The present invention relates to a method for producing a sputtering target material having high strength and uniform performance.
近年、耐熱材料やＨＤＤ用ターゲット材の新しい高融点金属を含有する合金が出現し、その製造方法としては、鋳造法および粉末成形法が試みられている。前者である鋳造法は最も一般的に使用される安価な方法であるが、組織の微細性や均質性で劣る。また、酸化物（ＳｉＯ2 、ＺｒＯ2 ）が入ったものなど高融点のターゲット材に対応できない。さらに、後者である粉末成形法は鋳造法に比べて高価であるが、組織が微細で組成も均質であるため作製される膜の品質が高いが、粉末を製造するに当たり、高融点の粉末を製造することが困難であるという、それぞれの欠点を持っている。 In recent years, alloys containing new refractory metals such as heat-resistant materials and HDD target materials have appeared, and casting methods and powder molding methods have been attempted as methods for producing the alloys. The former casting method is the most commonly used and inexpensive method, but is inferior in the fineness and homogeneity of the structure. Moreover, it cannot respond to a target material having a high melting point such as an oxide (SiO 2 , ZrO 2 ). Furthermore, the latter powder molding method is more expensive than the casting method, but the quality of the produced film is high because the structure is fine and the composition is homogeneous, but when producing the powder, a high melting point powder is used. Each has the disadvantage of being difficult to manufacture.
一方、ターゲット材に用いられる組成は金属や酸化物も含めて多岐に渡るが、金属元素単体のターゲット材は少なく、大部分は２元素以上の金属、もしくは金属合金と酸化物の複合体となっている。粉末法でこのような２元素以上からなる材料を作製する場合、狙い組成の合金粉末をあらかじめアトマイズ法などにより作製し、これをＨＩＰ（熱間等方圧プレス）やＨＰ（ホットプレス）等で成形する。しかし、この方法ではその合金が高融点でありアトマイズが困難である場合は作製することができない。 On the other hand, the composition used for the target material is diverse, including metals and oxides. However, there are few target materials consisting of metal elements alone, and most of them are composites of metals with two or more elements, or metal alloys and oxides. ing. When producing such a material consisting of two or more elements by a powder method, an alloy powder having a target composition is prepared in advance by an atomizing method or the like, and this is performed by HIP (hot isostatic pressing), HP (hot pressing) or the like. Mold. However, this method cannot be produced when the alloy has a high melting point and is difficult to atomize.
また、純金属同士を所定組成になるように混合し、これをＨＩＰ（熱間等方圧プレス）やＨＰ（ホットプレス）等で成形する方法もある。この方法では、成形時の加熱のみでは均一に合金化せず偏析の要因となる。このように偏析の存在するターゲット材をスパッタした場合、出来た薄膜の成分均質性が失われてしまう。また、２元素間に脆性相が存在するような合金系においては高温での成形時にその脆性相が析出し、これが原因で成形時に割れが発生するため好ましくない。 There is also a method in which pure metals are mixed so as to have a predetermined composition, and this is molded by HIP (hot isostatic pressing), HP (hot pressing) or the like. In this method, heating only at the time of forming does not form a uniform alloy but causes segregation. Thus, when the target material with segregation is sputtered, the homogeneity of the components of the resulting thin film is lost. Further, in an alloy system in which a brittle phase exists between two elements, the brittle phase precipitates at the time of molding at a high temperature, and this causes a crack at the time of molding, which is not preferable.
一例として、Ｃｒ−Ｍｎ系合金のターゲット材を作製しようとした場合、純Ｃｒと純Ｍｎを混合して成形すると、一部脆性相（σ）が析出し、これが原因で成形時に割れが発生したり、スパッタ時にその脆性部が欠落してスパッタ不良を起こしたりする。これを解決する方法として、例えば特開２００２−２１２６０７号公報（特許文献１）に開示されているように、ＨＩＰ法に替えて熱間押出法によって簡易に高圧が得られるこの方法で均一な単相を得る方法が提案されている。 As an example, when a target material of a Cr-Mn alloy is to be produced, when a mixture of pure Cr and pure Mn is formed, a brittle phase (σ) is partially precipitated, which causes cracks during forming. Or the brittle part is lost during sputtering, resulting in poor sputtering. As a method for solving this problem, as disclosed in, for example, Japanese Patent Application Laid-Open No. 2002-212607 (Patent Document 1), a high pressure can be easily obtained by a hot extrusion method instead of the HIP method. A method for obtaining the phase has been proposed.
また、特開２００３−１６７３２４号公報（特許文献２）に開示されているように、金属粉末あるいは水素化金属粉末とＳｉ粉末を混合し、これを加熱合成して金属シリサイド粉末とした後、この金属シリサイド粉末を機械的に微粉砕し、この微粉砕金属シリサイド粉末と微細Ｓｉ粉とを所定のモル比となるように均一混合し真空加熱炉を用いて焼成した金属シリサイド粉を焼結する金属シリサイドスパッタリングターゲットの製造方法が提案されている。 Further, as disclosed in Japanese Patent Application Laid-Open No. 2003-167324 (Patent Document 2), a metal powder or a metal hydride powder and a Si powder are mixed and heated to synthesize a metal silicide powder. Metal which pulverizes metal silicide powder mechanically, and sinters metal silicide powder which is pulverized using vacuum heating furnace after uniformly mixing the finely pulverized metal silicide powder and fine Si powder to a predetermined molar ratio. A method for manufacturing a silicide sputtering target has been proposed.
しかしながら、上述した特許文献１の熱間押出法によって簡易に高圧が得られる方法ではあるが、純金属粉末同士での形成であり、どうしても偏析の生じることは避けられない。また、特許文献２の焼結方法では合金系によっては脆性相が析出し、割れの要因となったり、ターゲット材として強度が落ちるという問題がある。
However, although it is a method in which high pressure can be easily obtained by the hot extrusion method of
上述のような問題を解消するために、発明者らは鋭意開発を進めた結果、合金粉末を使用することにより、純金属粉末同士を形成するよりも偏析が小さく、また金属間化合物（脆性相）が生成しない領域を選択して成形することにより割れの少ないターゲット材としての強度を向上させたスパッタリングターゲット材の製造方法を提供するものである。 In order to solve the above-mentioned problems, the inventors have intensively developed, and as a result, by using alloy powder, segregation is smaller than that formed between pure metal powders, and intermetallic compounds (brittle phase) The present invention provides a method for producing a sputtering target material in which the strength as a target material with few cracks is improved by selecting and molding a region that does not generate ().
その発明の要旨とするところは、
（１）脆性相が存在する２元系合金において、脆性相が存在する２元系合金での純金属と合金粉末を混合するに当たり、２元系状態図より脆性相（金属間化合物）が生成しない領域を選択して純金属と固溶体の粉末を混合した後熱間加圧成形し、脆性相のない合金を製造することを特徴とするスパッタリングターゲット材の製造方法。
The gist of the invention is that
(1) In a binary alloy containing a brittle phase, a brittle phase (intermetallic compound) is generated from a binary phase diagram when mixing pure metal and alloy powder in a binary alloy containing a brittle phase. A method for producing a sputtering target material, comprising selecting a region not to be mixed, mixing pure metal and solid solution powder, and then hot pressing to produce an alloy having no brittle phase.
ここで２元系状態図より脆性相（金属間化合物）が生成するとは、純金属１と純金属２からなる２元系合金が、純金属１がα％（αは１〜９９の任意の値）で純金属２が（１００−α）％で脆性相（以下「合金１」という）を生成することをいう。また２元系状態図より脆性相が生成しない領域を選択とは、２元系合金が純金属１をα％未満で純金属２を（１００−α）％を含有する合金（以下「合金２」という）を用いるという意味である。更に２元系状態図より脆性相（金属間化合物）が生成しない領域を選択して純金属と固溶体の粉末とは、純金属１からなる粉末１と、合金２が純金属１と合金０の固溶体である合金２からなる粉末２の両方を指す意味である。
Here, the generation of a brittle phase (intermetallic compound) from the binary phase diagram means that the binary alloy composed of
以上述べたように、本発明による合金粉末を使用することにより、純金属粉末同士を成形するよりも偏析が小さく、かつ脆性相が存在せず、しかも割れもなく高強度で均質なターゲット材の作製が可能となる極めて優れた効果を奏するものである。 As described above, by using the alloy powder according to the present invention, the segregation is smaller than that formed between pure metal powders, the brittle phase does not exist, and there is no crack, and the high strength and homogeneous target material is obtained. There is an extremely excellent effect that can be produced.
以下、本発明について図面に従って詳細に説明する。
図１は、本発明に係るＡ−Ｅ金属状態図である。この図に示すように、Ａ−Ｅ金属状態図において脆性相がＣ固溶体とＤ固溶体間にある場合を示した金属状態図である。本発明の第１は、この図１に示すような脆性相が存在するＡ−Ｅ２元系状態図において、純金属Ａと固溶体Ｃの粉末を混合して、熱間加圧成形し、Ｂ組成の合金を製造することを特徴とするスパッタリングターゲット材の製造方法にある。
Hereinafter, the present invention will be described in detail with reference to the drawings.
FIG. 1 is an AE metal phase diagram according to the present invention. As shown in this figure, in the AE metal phase diagram, it is a metal phase diagram showing a case where the brittle phase is between the C solid solution and the D solid solution. In the first aspect of the present invention, in the A-E binary phase diagram in which a brittle phase is present as shown in FIG. 1, powders of pure metal A and solid solution C are mixed, hot pressed, and B composition The present invention is directed to a method for producing a sputtering target material characterized by producing an alloy of
図２は、本発明に係る他のＡ−Ｅ金属状態図である。この図に示すように、Ａ−Ｅ金属状態図において脆性相がＣ固溶体とＥ金属間にある場合を示した金属状態図である。本発明の第２は、この図２に示すような脆性相が存在するＡ−Ｅ２元系状態図において、Ｂ組成金属の融点がＡ−Ｅ２元系状態図で最大である場合に、純金属Ａ´固溶体と固溶体Ｃの粉末を混合して、熱間加圧成形し、合金化することを特徴とするスパッタリングターゲット材の製造方法にある。 FIG. 2 is another AE metal phase diagram according to the present invention. As shown in this figure, in the AE metal phase diagram, it is a metal phase diagram showing a case where the brittle phase is between the C solid solution and the E metal. The second aspect of the present invention is a pure metal in the case where the melting point of the B composition metal is maximum in the A-E binary phase diagram in the A-E binary phase diagram where the brittle phase is present as shown in FIG. A sputtering target material manufacturing method is characterized by mixing powders of A ′ solid solution and solid solution C, hot pressing and alloying.
図３は、ターゲット表面でのスパッタ現象を示す図である。この図に示すように、ターゲット材２にＡｒなどの不活性な物質である入射イオン３を高速で衝突させると、ターゲット材２の表面で原子や分子と衝突して種々の現象が起こる。この現象のうちで、ターゲット材２を構成する原子や分子が叩き出される過程をスパッタリングといい、この叩き出せれたスパッタ粒子４、マイナスイオン５、γ電子６、スパッタ粒子の逆戻り７および入射イオンの反射８並びに反跳粒子９等と同時に原子や分子を基板１上に付着させ薄膜を形成する技術をスパッタ法という。
FIG. 3 is a diagram showing a sputtering phenomenon on the target surface. As shown in this figure, when incident ions 3 which are inert substances such as Ar collide with the
本発明は、上述したスパッタリングのためのターゲット材の製造方法にある。この材料としては、例えばＣｒ−Ｍｎ系の例で言えば、０≦Ｃｒ≦６０原子％、残部Ｍｎからなる成形体を作製する際、一方にはＣｒ−５５原子％程度の固溶体からなる合金粉末を作製し、これに純Ｃｒを所定の組成になるように混合することにより、σ相の析出は抑えられる。脆性相が析出しないので成形時の割れもなく、ターゲットとしての強度も十分で組成均質性も高い。他にもＣｏ−Ｃｒ系、Ｆｅ−Ｃｒ系、Ｃｒ−Ｗ系、Ｃｒ−Ｓｉ系等、合金系に脆性相が存在し、かつ所望する組成域が固溶体領域であれば同様に活用できる。 This invention exists in the manufacturing method of the target material for sputtering mentioned above. As this material, for example, in the case of Cr—Mn type, when producing a molded body composed of 0 ≦ Cr ≦ 60 atomic% and the balance Mn, one side is an alloy powder composed of a solid solution of about Cr-55 atomic%. And mixing with pure Cr so as to have a predetermined composition can suppress the precipitation of the σ phase. Since the brittle phase does not precipitate, there is no cracking during molding, the strength as a target is sufficient, and the composition homogeneity is high. In addition, if a brittle phase is present in an alloy system such as a Co—Cr system, a Fe—Cr system, a Cr—W system, a Cr—Si system, and the desired composition region is a solid solution region, it can be similarly utilized.
以下、本発明について実施例によって具体的に説明する。
表１に示す原料粉末をガスアトマイズ粉末法により製造し、それぞれの原料粉末をＶ型混合機を用いて各組成に３０分間の混合を行なった後、熱間加圧成形によるＨＩＰおよびＨＰにより、成形圧：１００ＭＰａ、成形温度：１４７３Ｋの条件で成形し、その後徐冷して、成形体サイズ：直径１８０ｍｍ×高さ１０ｍｍのものを得た。その成形体の特性調査として、外観：割れ発生の有無（カラーチェックにより確認し、１０枚中１枚以上割れがあれば、割れありとして評価）を評価した。また、Ｘ線回折：構成相の同定（測定角度２０〜８０°、ターゲットＣｕｋα）により脆性相の有無を確認した。さらに、成分分析のバラツキ：ＥＰＭＡにより線分析（測定幅１ｍｍ）を行い、平均値を０とした時の平均高さを組成バラツキとして算出した。その結果を表１に示す。
Hereinafter, the present invention will be specifically described with reference to examples.
The raw material powders shown in Table 1 are manufactured by the gas atomization powder method, and each raw material powder is mixed with each composition for 30 minutes using a V-type mixer, and then molded by HIP and HP by hot pressing. Molding was performed under the conditions of pressure: 100 MPa, molding temperature: 1473 K, and then gradually cooled to obtain a molded body size: diameter 180 mm × height 10 mm. As a characteristic survey of the molded body, appearance: presence / absence of crack generation (confirmed by a color check and evaluated if there is a crack in one or more sheets out of 10 sheets) was evaluated. Moreover, the presence or absence of a brittle phase was confirmed by X-ray diffraction: identification of constituent phases (measurement angle 20 to 80 °, target Cukα). Further, component analysis variation: Line analysis (measurement width: 1 mm) was performed by EPMA, and the average height when the average value was 0 was calculated as composition variation. The results are shown in Table 1.
表１に示すように、Ｎｏ．１〜６は本発明例であり、Ｎｏ．７〜１０は比較例である。比較例Ｎｏ．７、８は純Ｃｒと純Ｍｎの混合によるものであり、いずれも割れが発生し、脆性相を有し、かつ組成バラツキの値が大きい。比較例９、１０は純Ｃｏと純Ｃｒとの混合によるものであり、これもＮｏ．７と同様に、いずれも割れが発生し、脆性相を有し、かつ組成バラツキの値が大きいことが分かる。 As shown in Table 1, no. 1 to 6 are examples of the present invention. 7 to 10 are comparative examples. Comparative Example No. 7 and 8 are due to the mixture of pure Cr and pure Mn, both of which cracks occur, have a brittle phase, and have a large composition variation. Comparative Examples 9 and 10 are obtained by mixing pure Co and pure Cr. As in FIG. 7 , it is found that all cracks occur, the brittle phase is present, and the value of composition variation is large.
これに対し、本発明例であるＮｏ．１〜６は各純Ｃｒ、Ｆｅと合金粉末との混合から成形された２元系合金であり、いずれの特性も優れていることが分かる。 In contrast to this, No. 1 to 6 are binary alloys formed by mixing each pure Cr , Fe and alloy powder, and it is understood that all the characteristics are excellent.
このように、純金属粉と合金粉での成形は、脆性相が存在する合金系において、固溶体が得られる組成領域で合金粉末を作製し、この粉末に純金属粉末もしくは別組織の固溶体を混合し目的の成分とした上で成形することにより、脆性相が存在せず、割れもなく高強度で均質なターゲット材の作製が可能となったものである。 As described above, in molding with pure metal powder and alloy powder, an alloy powder is produced in a composition region where a solid solution is obtained in an alloy system in which a brittle phase exists, and pure metal powder or a solid solution of another structure is mixed with this powder. However, molding with the desired components made it possible to produce a high strength and homogeneous target material without a brittle phase and without cracks.
１ 基板
２ ターゲット材
３ 入射イオン
４ スパッタ粒子
５ マイナスイオン
６ γ電子
７ スパッタ粒子の逆戻り
８ 入射イオンの反射
９ 反跳粒子
特許出願人 山陽特殊製鋼株式会社
代理人 弁理士 椎 名 彊
DESCRIPTION OF
Patent Applicant Sanyo Special Steel Co., Ltd.
Attorney Atsushi Shiina
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5248000B2 (en) * | 2006-09-11 | 2013-07-24 | 山陽特殊製鋼株式会社 | CoW-based target material and method for manufacturing the same |
| JP4811660B2 (en) * | 2006-11-30 | 2011-11-09 | 三菱マテリアル株式会社 | High Ga-containing Cu-Ga binary alloy sputtering target and method for producing the same |
| JP4957969B2 (en) * | 2007-11-12 | 2012-06-20 | 三菱マテリアル株式会社 | Method for producing Cu-In-Ga ternary sintered alloy sputtering target |
| JP5459494B2 (en) * | 2010-03-28 | 2014-04-02 | 三菱マテリアル株式会社 | Sputtering target for forming a magnetic recording medium film and method for producing the same |
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