JPH01108367A - Manufacturing method of sputtering target - Google Patents
Manufacturing method of sputtering targetInfo
- Publication number
- JPH01108367A JPH01108367A JP26317687A JP26317687A JPH01108367A JP H01108367 A JPH01108367 A JP H01108367A JP 26317687 A JP26317687 A JP 26317687A JP 26317687 A JP26317687 A JP 26317687A JP H01108367 A JPH01108367 A JP H01108367A
- Authority
- JP
- Japan
- Prior art keywords
- casting mold
- temp
- melt
- crucible
- poured
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005477 sputtering target Methods 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000005266 casting Methods 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 14
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 230000005496 eutectics Effects 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 24
- 239000000463 material Substances 0.000 abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 6
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- 238000007711 solidification Methods 0.000 abstract description 4
- 230000008023 solidification Effects 0.000 abstract description 4
- 238000004544 sputter deposition Methods 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 3
- 239000000155 melt Substances 0.000 abstract 5
- 238000000034 method Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 150000003624 transition metals Chemical class 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000010408 film Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003353 gold alloy Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- -1 rare earth transition metal Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本、発明はスパッタリング用ターゲットの製造法に関す
る。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing a sputtering target.
高密度記録媒体として近年希土類遷移金属系薄膜による
光磁気気録膜が実用化されている。この薄膜を作成する
一つの方法としてスパッタリングがある。このスパッタ
リングにおいて膜原料は、スパッタリング用ターゲット
として供給される。Magneto-optical recording films made of rare earth transition metal thin films have recently been put into practical use as high-density recording media. Sputtering is one method for creating this thin film. In this sputtering, the film raw material is supplied as a sputtering target.
スパッタリング用ターゲットの、製造法としては、鋳造
法、焼結法などがあるが、コストが安価であり含を酸素
量が少量であるという点から前者が優れている。Methods for producing sputtering targets include casting and sintering, but the former is superior because it is inexpensive and contains a small amount of oxygen.
光磁気気録膜の組成は種々あるが、性能、価格という点
から希土頂−遷移金属系合金が主流となり、希土類と遷
移金属の組成比がＣｍｏｌ比で）３ニア付近のものが多
用されている。There are various compositions for magneto-optical recording films, but rare earth-transition metal alloys are mainstream from the viewpoint of performance and price, and those with a composition ratio of rare earth and transition metal of around 3 (in terms of Cmol ratio) are often used. ing.
この合金系は、この組成比付近にて、希土類をＲ１遷移
金属をＴとすると、Ｒ，Ｔ、とＲｌＴｓの共晶系を為す
場合が多い。This alloy system often forms a eutectic system of R, T, and RlTs near this composition ratio, where R1 is the rare earth and T is the transition metal.
従来の技術においては、注湯の温度は、粘性のみを考慮
し、共晶系の初晶析出塩より高く設定されていた。In the conventional technology, the pouring temperature was set higher than that of the eutectic primary crystallized salt, considering only the viscosity.
しかし前述の注湯の温度にて鋳造した場合、前述の多用
される希土類−遷移金属系の合金においては、まず板状
の初晶が晶出し、次に第２品が晶出する。その原初晶は
、９ｓ２晶組成を持った溶湯を閉じ込めたセルを作る。However, when casting is carried out at the above-mentioned pouring temperature, in the case of the above-mentioned frequently used rare earth-transition metal alloy, plate-shaped primary crystals are first crystallized, and then second crystals are crystallized. The primordial crystal forms a cell that confines the molten metal with a 9S2 crystal composition.
この初晶の壁は、第２品組成の溶湯を隣接したセル中の
溶湯と完全に遮断することが多いため、第２晶が凝固す
る際、凝固収縮しても押し湯等が充分に補給されない、
そのためこの系の鋳造合金には多くの細かい引は栗が存
在する。このような引は巣の多く存在するスパッタリン
グ用ターゲットは、引は果部への応力集中による物理的
強度の低下、あるいは、スパッタリング時におけるプラ
ズマが不安定などの問題点を育する。The wall of this primary crystal often completely blocks the molten metal of the second product composition from the molten metal in the adjacent cell, so when the second crystal solidifies, even if it solidifies and shrinks, the riser etc. is sufficiently replenished. not be done,
Therefore, many fine grains exist in this type of cast alloy. A sputtering target with many such elongated cavities has problems such as a decrease in physical strength due to stress concentration on the elongated portions or unstable plasma during sputtering.
このような問題点を解決するためには、ルツボ中にて初
晶を晶出させてから鋳型に注湯するという鋳造方法があ
る。この方法によれば予め初晶からルツボ中の湯の撹拌
によりばらばらに晶出しているためそれをｔｓ型に注湯
、鋳造した場合初晶による完全に閉じたセルは作られな
い、従って第２晶晶出時に湯が良く行きわたり、凝固収
縮による小さな引は果はな（なる。しかし、この方法の
場合、ルツボ中にて析出した初晶がルツボ壁に付着し、
組成ずれが起き、また鋳造時の湯温が低いため注湯の粘
性が高く、ルツボ中に湯が残ってしまい、歩留りが悪い
という欠点を存する。特にスパッタリング用ターゲット
は、組成ずれはあってはいけな（、また材料が高価なも
のの場合が多いので歩留りは、大きくないといけなく、
このような欠点は大きな障害となってくる。そこで、本
発明は、このような問題点を解決するもので、その目的
とするところは、引は巣のなく歩留りの良い鋳造スパッ
タリング用ターゲットを供給するところにある。In order to solve these problems, there is a casting method in which primary crystals are crystallized in a crucible and then poured into a mold. According to this method, the primary crystals are preliminarily crystallized by stirring the hot water in the crucible, so when the primary crystals are poured into a TS mold and cast, a completely closed cell is not created by the primary crystals. During crystallization, the hot water spreads well and there are no small effects due to solidification shrinkage. However, in this method, the primary crystals precipitated in the crucible adhere to the crucible wall,
There is a disadvantage that compositional deviation occurs, and since the hot water temperature during casting is low, the viscosity of the poured metal is high, hot water remains in the crucible, and the yield is poor. In particular, sputtering targets must not have compositional deviations (and since the materials are often expensive, the yield must be high).
Such shortcomings become a major hindrance. SUMMARY OF THE INVENTION The present invention is intended to solve these problems, and its purpose is to provide a casting sputtering target that is free of cracks and has a high yield.
本発明のスパッタリング用ターゲットの製造法は、共晶
系を為す希土類−遷移金屑系合金を鋳造にてスパッタリ
ング用ターゲットとする原、ルツボと鋳型の中間にて注
湯の温度を、初晶析出温度以下、第２晶晶出温度以上と
し鋳型に注湯鋳造することを特徴とする。The method for manufacturing a sputtering target of the present invention involves casting a rare earth-transition gold alloy having a eutectic system to form a sputtering target, and adjusting the temperature of pouring between the crucible and the mold to induce primary crystal precipitation. It is characterized by pouring the molten metal into a mold at a temperature below the second crystallization temperature and above the second crystallization temperature.
本発明上記の鋳造法によれば、溶湯がルツボから出てか
ら初晶を晶出させ、第２晶組成の溶湯と混合状態とする
。この混合の半溶融状態の溶湯をｖｉ型に注ぎ込み鋳造
する。このとき初晶は湯の流動により撹拌され、片状と
なっておりｔＩＩＩＪｌ内部で閉じたセルは作らない、
従って鋳型冷却による第２品の凝固収縮に当っては、収
縮分は、押し湯によってすみやかに溶湯が供給される。According to the above-described casting method of the present invention, primary crystals are crystallized after the molten metal comes out of the crucible, and mixed with the molten metal having a secondary crystal composition. This mixed semi-molten metal is poured into a VI mold and cast. At this time, the primary crystals are stirred by the flow of hot water and become flaky and do not form closed cells inside tIIIJl.
Therefore, when the second product solidifies and shrinks by cooling the mold, the shrinkage is quickly replaced by molten metal by the riser.
従って第２品の凝固収縮による引は巣はほとんどな（な
る。Therefore, there are almost no cavities caused by solidification and shrinkage of the second product.
（実施例１）
鋳造材料としてＮｄｔ 、ｘ Ｄｙ＊ ｓ 、ａ Ｆｅ
。(Example 1) Ndt, x Dy* s, a Fe as casting materials
.
６ 、 ＠ ＣＯＨ４、。の４元素の材料を用いた。こ
の合金系は、上記組成近傍においては、希土類と遷移金
属の擬似２元素をなし、その鋳造物においては、Ｒ，Ｔ
、 、Ｒ，Ｔ、の２組が粉末Ｘｌ１１回折回折により同
定された。ここにおいてＲ，Ｔのそれぞれの中でＮｄと
Ｄｙ、ＦｅとＣｏがそれぞれ置換し合っており、例えば
ＤｙＦｅ、とＤｙＣ。6, @COH4,. A material containing four elements was used. This alloy system has pseudo-binary elements of rare earth and transition metal in the vicinity of the above composition, and in its casting, R, T
, , R, T, were identified by powder Xl11 diffraction diffraction. Here, in each of R and T, Nd and Dy, and Fe and Co are substituted with each other, for example, DyFe and DyC.
、が別々に分離して存在することは認められなかった。, were not allowed to exist separately.
第１図に本発明の鋳造法の模式断面図を示し、鋳造方法
に沿って説明をする。FIG. 1 shows a schematic sectional view of the casting method of the present invention, and the casting method will be explained.
上述材料は、ルツボ１０１中にて、真空溶解する。この
ルツボを傾は中の溶湯１０４をタンデイシュ１０２を通
じて鋳型１０３に注湯する。タンデイシュは、熱伝導率
の良い材料で製作しであるため、溶湯１０４は、タンデ
イシュを通過する際に初晶晶出温度以下となり初晶が晶
出する。この除温の粘性はかなり高くなるのでタンデイ
シュの湯の当る表面は平面で構成した方が良い。このよ
うにして初晶が晶出した半溶融伏顛の湯は＃型に流し込
まれる。初晶はタンデイシュを通過する際等の撹拌によ
りばらばらの片状となっており、鋳型中では閉じたセル
を作らず第２品晶出時の押し湯はすみやかに供給され凝
固収縮に起因する小さな引は巣は存在しな（なる。The above-mentioned materials are melted in a vacuum in the crucible 101. The crucible is tilted and the molten metal 104 inside is poured into the mold 103 through the tundish 102. Since the tundish is made of a material with good thermal conductivity, the temperature of the molten metal 104 becomes lower than the primary crystallization temperature when passing through the tundish, and primary crystals crystallize. The viscosity of this temperature removal process is quite high, so it is better to make the surface of the tundish that comes into contact with the hot water flat. The semi-molten hot water in which the primary crystals have crystallized in this way is poured into the # mold. The primary crystals are in the form of separate pieces due to agitation when passing through the tundish, and do not form closed cells in the mold. The nest doesn't exist.
（比較例１） 上記（実施例１）と同材料で溶解鋳造した。(Comparative example 1) The same material as above (Example 1) was melted and cast.
（実施例１）と違う点はタンデイシュを熱伝導度が悪く
熱容量が小さい、発砲状セラミックスを使用した点であ
る。このタンデイシュ使用のため溶湯は、初晶晶出温度
以下にならず、初晶は鋳型中で晶出し、閉じたセルを作
った。The difference from Example 1 is that the tundish is made of foamed ceramic, which has poor thermal conductivity and small heat capacity. Because of the use of this tundish, the molten metal did not drop below the primary crystallization temperature, and the primary crystals crystallized in the mold to form closed cells.
上記（実施例１）と、（比較例１）で作成したターゲッ
ト用鋳塊を比較してるると（実施例りには引は巣はほと
んど存在しないが（比較例１）には細かい収縮孔が多く
存在する。Comparing the target ingots prepared in Example 1 and Comparative Example 1 above, there are almost no shrinkage cavities in Example 1, but fine shrinkage holes in Comparative Example 1. There are many.
（実施例２）
鋳造材料としてＴｂｔ ａ Ｆ ｅｔ ｘ （ｍｏ
Ｉ比）を使用したＴｂ−Ｆｅ系において上記の組成の合
金は、Ｔｂｙ Ｔｂｊ、Ｔｂｓ Ｆｅ、の共晶系を為す
。それぞれの融点が１２１２℃、１１８７℃を示す。Ｊ
ＬＣＭ；４５ （１９７８）、ＰＰ、９１−１０１゜
上記組成を（実施例１）と同じ方法にて鋳造した。(Example 2) Tbt a F et x (mo
In the Tb-Fe system using the I ratio), the alloy with the above composition forms a eutectic system of Tby Tbj, Tbs Fe. The respective melting points are 1212°C and 1187°C. J
LCM; 45 (1978), PP, 91-101° The above composition was cast in the same manner as in Example 1.
（比較例２）
鋳造材料としてＴＩ）＊ ＊ Ｆ ｅｔ ｔ （ｍｏ
ｌ比）を使用して（比較例１）と同じ方法にて鋳造を
行なった。(Comparative Example 2) TI) * * F et t (mo
Casting was carried out in the same manner as in Comparative Example 1 using the same ratio as in Comparative Example 1.
（実施例２）と（比較例２）を比較してみると実施例２
には、引は巣がほとんどないのに対して比較例２には、
第２晶晶出時の細かい収縮孔が多く存在する。Comparing (Example 2) and (Comparative Example 2), Example 2
There are almost no nests in Comparative Example 2.
There are many fine shrinkage pores during the second crystallization.
尚、本実施例においては、希土類と遷移金属の比を３ニ
アにしたため、初晶がＲ，Ｔ、となったが、これより遷
移金属が多い場合、少ない場合がある。このような時本
合金系は多くの共晶系をなすが、本方法はいずれの場合
にても育効ｔある。In this example, the ratio of rare earth and transition metal was set to 3-nea, so the primary crystals were R and T. However, if the transition metal is more than this, it may be less. In such cases, the present alloy system forms many eutectic systems, and the present method is effective for growth in any case.
また、初晶を晶出するために本実施例においては、タン
デイシュを用いたが、タンデイシュまでの途中に、冷却
能のある樋などを設置し、そこを湯を通すことにより湯
を冷却する方法も宵効である。In addition, in this example, a tundish was used to crystallize the primary crystals, but there is a method in which a gutter with a cooling capacity is installed on the way to the tundish, and the hot water is cooled by passing the hot water through it. It is also in effect.
以上述べたように発明によれば、共晶系を為す希土類−
遷移金属系合金を鋳造にてスパッタリング用ターゲット
とする際、ルツボと鋳型の中間にて、注湯の温度を、初
晶晶出温度以下、第２晶晶出温度以上とし鋳型に注湯、
鋳造することにより細かい第２品晶出時の凝固収縮孔を
なくすという効果を育する。As described above, according to the invention, rare earths forming a eutectic system -
When casting a transition metal alloy to use as a sputtering target, pour the metal into the mold at a temperature that is below the primary crystallization temperature and above the secondary crystallization temperature at an intermediate point between the crucible and the mold.
Casting has the effect of eliminating solidification shrinkage pores during crystallization of the fine second product.
第１図は、本発明の鋳造法の模式断面図。 １０１・・・溶解ルツボ １０２・・・タンデイシュ １０３・・・鋳型 １０４・・・溶湯 以 上 出願人 セイコーエプソン株式会社 FIG. 1 is a schematic cross-sectional view of the casting method of the present invention. 101... Melting crucible 102...Tandish 103...Mold 104...molten metal that's all Applicant: Seiko Epson Corporation
Claims (1)
タリング用ターゲットとする際、ルツボと鋳型の中間に
て、注湯の温度を初晶晶出温度以下、第２晶晶出温度以
上とし鋳型に注湯、鋳造することを特徴とするスパッタ
リング用ターゲットの製造法。When casting a rare earth-transition metal alloy that forms a eutectic system to use as a sputtering target, the temperature of pouring the metal between the crucible and the mold is set to be below the primary crystallization temperature and above the secondary crystallization temperature. A method of manufacturing a sputtering target characterized by pouring the metal into a mold and casting it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26317687A JPH01108367A (en) | 1987-10-19 | 1987-10-19 | Manufacturing method of sputtering target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26317687A JPH01108367A (en) | 1987-10-19 | 1987-10-19 | Manufacturing method of sputtering target |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01108367A true JPH01108367A (en) | 1989-04-25 |
Family
ID=17385827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26317687A Pending JPH01108367A (en) | 1987-10-19 | 1987-10-19 | Manufacturing method of sputtering target |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01108367A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0570933A (en) * | 1991-03-19 | 1993-03-23 | Mitsubishi Materials Corp | Manufacture of slender bar-like raw material for vapor-deposition |
-
1987
- 1987-10-19 JP JP26317687A patent/JPH01108367A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0570933A (en) * | 1991-03-19 | 1993-03-23 | Mitsubishi Materials Corp | Manufacture of slender bar-like raw material for vapor-deposition |
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