JPS61124564A - Formation of thin film - Google Patents

Formation of thin film

Info

Publication number
JPS61124564A
JPS61124564A JP24343084A JP24343084A JPS61124564A JP S61124564 A JPS61124564 A JP S61124564A JP 24343084 A JP24343084 A JP 24343084A JP 24343084 A JP24343084 A JP 24343084A JP S61124564 A JPS61124564 A JP S61124564A
Authority
JP
Japan
Prior art keywords
thin film
alloy
target
sputtering
homogeneous
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
Application number
JP24343084A
Other languages
Japanese (ja)
Inventor
Tetsuo Hashii
橋井 哲雄
Hiroyoshi Ishii
石井 博義
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Riken Corp
Original Assignee
Riken Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Riken Corp filed Critical Riken Corp
Priority to JP24343084A priority Critical patent/JPS61124564A/en
Publication of JPS61124564A publication Critical patent/JPS61124564A/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
    • H01F41/183Sputtering targets therefor

Abstract

PURPOSE:To form the thin film of an alloy having uniform quality consisting of two or more kinds of elements by sputtering by using an amorphous alloy obtd. by quenching the molten of the alloy for forming thin film as a target. CONSTITUTION:The thin film of an alloy consisting of two or more kinds of elements is formed on the surface of a substrate by sputtering. At this time, a ribbonlike target contg. >=60% amorphous part is used as a target for sputtering. The ribbonlike target is produced by super quenching a molten alloy contg. two or more kinds of elements fed onto a rapidly moving cooling surface at 10<5>-10<6> deg.C/sec cooling rate. The thin film of the alloy having a uniform composition can be easily formed on a substrate by sputtering with the resulting target.

Description

【発明の詳細な説明】 (イ)発明の技術分野 この発明は、プラズマスパッタリング法あるいはイオン
ビームスパッタリング法などの物理蒸着法により、二種
以上の構成元素を含み且つ均質である薄膜を形成する方
法に関する。
Detailed Description of the Invention (a) Technical Field of the Invention This invention relates to a method for forming a homogeneous thin film containing two or more constituent elements by a physical vapor deposition method such as a plasma sputtering method or an ion beam sputtering method. Regarding.

(ロ)従来技術と問題点 近年、プラズマスパッタリング法あるいはイオンビーム
スパッタリング法等の物理蒸着法による薄膜形成技術が
、磁気バルブ、光磁気デスクメモリー、磁気転写素子、
垂直磁気記録など電子工業分野を中心に発展してきてい
る。
(b) Prior art and problems In recent years, thin film forming technology using physical vapor deposition methods such as plasma sputtering method or ion beam sputtering method has been used for magnetic valves, magneto-optical disk memories, magnetic transfer elements, etc.
It has been developing mainly in the electronic industry field, such as perpendicular magnetic recording.

この種の蒸着薄膜を工業的に利用する場合には、その薄
膜の微小領域での組織の不均一はそのまま薄膜の特性に
影響するため、高純度であり特に均質な薄膜が要求され
る。
When this type of vapor-deposited thin film is to be used industrially, a highly pure and particularly homogeneous thin film is required, since the non-uniformity of the structure in minute regions of the thin film directly affects the properties of the thin film.

ところで、一種類の構成元素からなる蒸着薄膜を高純度
で且つ均質な状態で得る技術は従来かなり進歩しており
比較的容易に得ることができる。
By the way, the technology for obtaining a vapor-deposited thin film made of one type of constituent element in a highly pure and homogeneous state has been considerably advanced and can be obtained relatively easily.

しかしながら、二種以上の構成元素を含む蒸着薄膜を十
分に均質な状態で得るにはいくつかの問題がある。例え
ば、二種以上の構成元素を含む蒸着薄膜を従来のスパッ
リングの方法に従って形成させる場合、得られる薄膜は
、一般に、結晶質と非晶質との混合相でなる薄膜となり
易く、十分に均質な薄膜を得ることは困難であった。
However, there are several problems in obtaining a deposited thin film containing two or more constituent elements in a sufficiently homogeneous state. For example, when a vapor-deposited thin film containing two or more constituent elements is formed according to the conventional sputtering method, the obtained thin film generally tends to be a thin film consisting of a mixed phase of crystalline and amorphous, and is sufficiently homogeneous. It has been difficult to obtain a thin film with good results.

微視的な不均質にせよ薄膜に生ずるこのような組織の不
均一はそのまま薄膜の特性に影響するために更に均質な
薄膜の形成方法の開発が望まれていた。
Even microscopic non-uniformity in the structure of a thin film directly affects the properties of the thin film, so it has been desired to develop a method for forming a more homogeneous thin film.

(ハ)発明の目的 この発明は、上記に鑑み、二種以上の物質を含み且つ均
質である薄膜を得ることを可能にする薄膜の形成方法を
提供することを目的としてなされたものである。
(c) Purpose of the Invention In view of the above, the present invention has been made with the object of providing a method for forming a thin film that makes it possible to obtain a homogeneous thin film containing two or more types of substances.

(ニ)発明の構成及び効果 この発明は、二種以上の元素を含む合金薄膜を形成する
スパッリング法において、前記薄膜を構成する物質を溶
融して均質な溶融状態の合金となし、次いで該溶融合金
を移動する冷却面に供給して急冷凝固させて均一な組織
とした超急冷材料をターゲツト材として用いることを特
徴とする薄膜形成方法に係る。
(D) Structure and Effects of the Invention The present invention provides a sputtering method for forming an alloy thin film containing two or more types of elements, in which a substance constituting the thin film is melted to form an alloy in a homogeneous molten state, and then the The present invention relates to a thin film forming method characterized by using as a target material an ultra-quenched material in which a molten alloy is supplied to a moving cooling surface and rapidly solidified into a uniform structure.

本発明では、二種以上の元素を構成元素として含む合金
薄膜を物理蒸着法によって形成するに用いられるターゲ
ツト材は、溶融されて均一な融体とさた溶融合金を、移
動する冷却面に供給して急冷凝固させる所謂液体急冷法
によって製造される材料でなっている。上記の液体急冷
法で得られた材料は、融体からの冷却速度が10’〜1
0”C/880以上であるため、非晶質合金あるいは非
平衡状態の結晶質合金となり極めて均質なものとなる。
In the present invention, the target material used to form an alloy thin film containing two or more elements as constituent elements by physical vapor deposition is a method in which the molten alloy is melted into a uniform melt and is supplied to a moving cooling surface. It is made of a material manufactured by the so-called liquid quenching method, in which it is rapidly cooled and solidified. The material obtained by the above liquid quenching method has a cooling rate of 10' to 1
Since it is 0''C/880 or more, it becomes an amorphous alloy or a crystalline alloy in a non-equilibrium state and becomes extremely homogeneous.

即ち、非晶質状態となった場合は、各構成原子が等方的
にランダムに均一混合した状態となっており、また、非
平衡状態の結晶質となった場合においてもその結晶粒度
は従来の溶製方法による場合に較べて格段に微細なもの
となり偏析の極めて少ない均質なものとなっている。
In other words, when it becomes an amorphous state, the constituent atoms are isotropically and randomly mixed uniformly, and even when it becomes a crystalline state in a non-equilibrium state, its crystal grain size remains the same as before. Compared to the case using the melting method, it is much finer and homogeneous with extremely less segregation.

上記の本発明の薄膜形成方法においては、スバ)クリン
グ法により形成される薄膜の母材となるターゲツト材が
高度に均質化されている。したがって、本発明方法によ
って得られる薄膜は、従来の合金ターゲツト材を使用し
て得られる薄膜に較べて均質なものとなる。なお、液体
急冷材は、通常、粉末あるいはリボン状として得られる
が、これらをターゲツト材として使用する場合、コール
ドプレス法、ホットプレス法、HIP、CIPあるいは
衝撃圧着法等の任意の方法により成形して使用すること
ができる。
In the thin film forming method of the present invention described above, the target material, which is the base material of the thin film formed by the subcling method, is highly homogenized. Therefore, the thin films obtained by the method of the present invention are more homogeneous than those obtained using conventional alloy target materials. The liquid quenching material is usually obtained in the form of powder or ribbon, but when used as a target material, it can be molded by any method such as cold pressing, hot pressing, HIP, CIP, or impact bonding. can be used.

(実施例−1) 原子%でSi5%、810%、残をFeとする合金を溶
融して均一な融体とし、この融体を対向して高速回転す
るロール間の間隙に噴流として供給し該噴流を分断し、
更にこれを回転する冷却円板に当てて急冷凝固させる液
体急冷法(キャビテーション法)により合金粉末を作成
した。
(Example-1) An alloy containing 5% Si, 810% Si, and the balance Fe in atomic % is melted to form a uniform melt, and this melt is supplied as a jet to the gap between opposing rolls rotating at high speed. dividing the jet,
Furthermore, an alloy powder was created by a liquid quenching method (cavitation method) in which the powder was applied to a rotating cooling disk and rapidly solidified.

得られた合金粉末は、X線解析の結果、非晶質と微細な
結晶質との混在した構造を呈していることが確認された
As a result of X-ray analysis, it was confirmed that the obtained alloy powder had a mixed structure of amorphous and fine crystalline materials.

この粉末をCIP法により径20III11で高さ5m
+oに成形しターゲツト材(本発明材)とした。また、
比較のために前記合金と同一組成の合金を溶融し、従来
のC○2&!型に注湯し前記と同一形状のターゲツト材
(比較材)を得た。得られた各ターゲツト材の組織写真
をそれぞれ第1図および第2図に示す。
This powder was prepared using the CIP method to a diameter of 20III11 and a height of 5m.
It was molded into +o and used as a target material (material of the present invention). Also,
For comparison, an alloy with the same composition as the above alloy was melted and the conventional C○2 &! Molten metal was poured into a mold to obtain a target material (comparative material) having the same shape as above. Photographs of the structure of each target material obtained are shown in FIGS. 1 and 2, respectively.

第1図、第2図より明らかなように、本発明で使用され
るターゲツト材(本発明材)の組織は均一であり、比較
材の全屈組織は混合組織をなしている。 これらのター
ゲツト材を用いて、高周波スパッタリング装置で、電極
間距離6co+、出力20OW、雰囲気2 X 10−
” Torrのアルゴンガスの条件で、ガラス基板に厚
さlo、oooAのスパッター膜を形成した。
As is clear from FIGS. 1 and 2, the target material used in the present invention (present invention material) has a uniform structure, and the comparative material has a mixed structure. Using these target materials, a high frequency sputtering device was used with a distance between electrodes of 6co+, an output of 20OW, and an atmosphere of 2×10−.
” A sputtered film with a thickness of lo and oooA was formed on a glass substrate under argon gas conditions of Torr.

得られたスパッター膜についてX線回折を行ったところ
ターゲツト材(本発明材)を使用した場合には完全な非
晶質の薄膜となり(第3図参照)、比較のターゲツト材
(比較材)を使用した場合には非晶質と結晶質とが温材
する薄膜が形成された(第4図参照)。
X-ray diffraction was performed on the resulting sputtered film, and when the target material (invention material) was used, it became a completely amorphous thin film (see Figure 3). When used, a thin film of amorphous and crystalline materials was formed (see FIG. 4).

(実施例−2) 原子%で、 Gd 25%、残COよりなる組成の合金
を溶融して均一な融体とし、これを高速回転するロール
面に供給して急冷凝固させる液体急冷法により厚さ0.
04 mm、巾3011IIOのリボン状素材を得た。
(Example-2) An alloy having a composition consisting of 25% Gd and residual CO in atomic % is melted to form a uniform melt, and this is supplied to a roll surface rotating at high speed to rapidly solidify it. Sa0.
A ribbon-like material having a diameter of 0.04 mm and a width of 3011 IIO was obtained.

これを積層して固着し、径20mm、厚さ51のターゲ
ツト材を作成した。
This was laminated and fixed to create a target material with a diameter of 20 mm and a thickness of 51 mm.

このターゲツト材を用いて、高周波スパッタリング装置
で、電極間距離6 cm、出力200W、雰囲気2 X
 1O−2Torrのアルゴンガスの条件でガラス基板
上に厚さ10,000人のスパッター膜を形成した。
Using this target material, a high frequency sputtering device was used with a distance between electrodes of 6 cm, an output of 200 W, and an atmosphere of 2
A sputtered film with a thickness of 10,000 yen was formed on a glass substrate under argon gas conditions of 10-2 Torr.

得られた蒸着膜は、X線回折の結果、均質な非晶質であ
った。
As a result of X-ray diffraction, the obtained deposited film was found to be homogeneous and amorphous.

(実施例−3) 原子%で、C11%、 Si 2%残部Feよりなる組
成の合金を液体急冷法にて前記同様なリボンを作成し、
これを乳鉢で粉砕し、ホットプレスにより成形し径10
0+m、厚さ10■■のターゲツト材とした。
(Example 3) A ribbon similar to the above was prepared by a liquid quenching method using an alloy having a composition of 11% C, 2% Si, and the balance Fe in terms of atomic percent.
This was crushed in a mortar and molded with a hot press to a diameter of 10 mm.
The target material was 0+m and 10mm thick.

このターゲツト材を使用し、高周波スパッタリング装置
により、電極間距離6cI11、出力200W。
Using this target material, the distance between the electrodes was 6cI11 and the output was 200W using a high frequency sputtering device.

雰囲気2 X 1O−2Torrのアルゴンガスの条件
においてガラス基板上に厚さ1s、ooo iのスパッ
ター膜を形成した。得られた薄膜についてX線回折の結
果、極めて均質な非晶質の薄膜であった。
A sputtered film having a thickness of 1 s and an ooo i was formed on a glass substrate under the conditions of an argon gas atmosphere of 2 x 10-2 Torr. As a result of X-ray diffraction of the obtained thin film, it was found to be an extremely homogeneous amorphous thin film.

以上の通りで、本発明では2種以上の構成元素を含有す
る薄膜をプラズマスパッタリング法、イオンビームスパ
ッタリング法などの物理蒸着法ににより形成する場合に
使用するターゲツト材として、該構成元素を含む物質を
溶融し、該融体を超急冷凝固させてる所謂液体急冷方法
の技術を利用して製造されたターゲツト材を使用するこ
とにより均質なスパッター膜を得ることを可能にしたも
のであり、その工業的価値は大である。
As described above, in the present invention, a substance containing two or more constituent elements is used as a target material when forming a thin film containing two or more constituent elements by a physical vapor deposition method such as a plasma sputtering method or an ion beam sputtering method. This technology has made it possible to obtain a homogeneous sputtered film by using a target material manufactured using the so-called liquid quenching method, in which the molten material is melted and solidified by ultra-rapid cooling. The value is great.

なお、上記の実施例では非晶質のスパッター膜を得る例
について示したが、本発明方法でにより結晶質の薄膜を
得ようとする場合には、上記実施例に従い得られた非晶
質薄膜を昇温しで結晶化させることにより均質な結晶質
薄膜とすることができる。
In addition, although the above example shows an example of obtaining an amorphous sputtered film, when attempting to obtain a crystalline thin film by the method of the present invention, the amorphous thin film obtained according to the above example may be used. By crystallizing it by raising the temperature, a homogeneous crystalline thin film can be obtained.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明で用いるターゲツト材の実施例を示す顕
微鏡組織写真(X200)、第2@は従来の方法で製造
したターゲツト材の顕微鏡組織写真(x zoo)。第
3図は本発明方法で得られたスパッター膜のX線回折チ
ャート図、第4図は従来のターゲツト材を用いて得られ
たスパッター膜のX線回折チャート図。
Fig. 1 is a microscopic structure photograph (X200) showing an example of the target material used in the present invention, and Fig. 2 is a microscopic structure photograph (x zoo) of a target material manufactured by a conventional method. FIG. 3 is an X-ray diffraction chart of a sputtered film obtained by the method of the present invention, and FIG. 4 is an X-ray diffraction chart of a sputtered film obtained using a conventional target material.

Claims (1)

【特許請求の範囲】 1)2種以上の構成元素を含む薄膜を形成するスパッタ
リング法において、該構成元素を含む物質を溶融し均質
な融体とし、該融体を移動する冷却面に供給して急冷凝
固させて均一な組織とした超急冷材料をターゲット材料
として使用することを特徴とする均質な薄膜の形成方法
。 2)前記超急冷材料の60%以上が非晶質である特許請
求の範囲第1項記載の薄膜の形成方法。
[Claims] 1) In a sputtering method for forming a thin film containing two or more constituent elements, a substance containing the constituent elements is melted into a homogeneous melt, and the melt is supplied to a moving cooling surface. A method for forming a homogeneous thin film, characterized in that an ultra-quenched material that is rapidly solidified into a uniform structure is used as a target material. 2) The method of forming a thin film according to claim 1, wherein 60% or more of the ultra-quenched material is amorphous.
JP24343084A 1984-11-20 1984-11-20 Formation of thin film Pending JPS61124564A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP24343084A JPS61124564A (en) 1984-11-20 1984-11-20 Formation of thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24343084A JPS61124564A (en) 1984-11-20 1984-11-20 Formation of thin film

Publications (1)

Publication Number Publication Date
JPS61124564A true JPS61124564A (en) 1986-06-12

Family

ID=17103753

Family Applications (1)

Application Number Title Priority Date Filing Date
JP24343084A Pending JPS61124564A (en) 1984-11-20 1984-11-20 Formation of thin film

Country Status (1)

Country Link
JP (1) JPS61124564A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009242947A (en) * 2003-08-05 2009-10-22 Nippon Mining & Metals Co Ltd Sputtering target and method for production thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009242947A (en) * 2003-08-05 2009-10-22 Nippon Mining & Metals Co Ltd Sputtering target and method for production thereof
JP2009263795A (en) * 2003-08-05 2009-11-12 Nippon Mining & Metals Co Ltd Sputtering target and method for production thereof
JP2009263796A (en) * 2003-08-05 2009-11-12 Nippon Mining & Metals Co Ltd Sputtering target and method for production thereof

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