JPH0364585B2 - - Google Patents
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- Publication number
- JPH0364585B2 JPH0364585B2 JP26710686A JP26710686A JPH0364585B2 JP H0364585 B2 JPH0364585 B2 JP H0364585B2 JP 26710686 A JP26710686 A JP 26710686A JP 26710686 A JP26710686 A JP 26710686A JP H0364585 B2 JPH0364585 B2 JP H0364585B2
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- JP
- Japan
- Prior art keywords
- alloy
- less
- present
- cao
- vapor deposition
- 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.)
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- 239000000956 alloy Substances 0.000 claims description 54
- 229910045601 alloy Inorganic materials 0.000 claims description 52
- 238000007740 vapor deposition Methods 0.000 claims description 23
- 230000008021 deposition Effects 0.000 claims description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 24
- 235000012255 calcium oxide Nutrition 0.000 description 23
- 239000000292 calcium oxide Substances 0.000 description 23
- 230000005291 magnetic effect Effects 0.000 description 23
- 239000010409 thin film Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 17
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 13
- 238000004544 sputter deposition Methods 0.000 description 13
- 238000000151 deposition Methods 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000011572 manganese Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000011819 refractory material Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 229910001004 magnetic alloy Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052661 anorthite Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000005247 gettering Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Description
［産業上の利用分野］
本発明は蒸着用Mn−Sb基合金に係り、特に磁
気記録材料として用いられる薄膜の製造に好適な
蒸着用Mn−Sb基合金に関する。
［従来の技術］
非磁性基板上に磁性合金薄膜を形成した磁気記
録材料は周知である。
この磁気記録材料の薄膜を製造する方法として
は、スパツタリングや真空蒸着、イオンプレーテ
イング党の蒸着法が広く用いられている。
特に、スパツタリング法は、均一な内部組成で
一定の合金元素を含んだターゲツト材が得られさ
えすれば、スパツタリング装置内の圧力をコント
ロールしながら組成的に均一な薄膜を得ることが
できる点で有利である。
磁性合金薄膜を形成する強磁性合金としては、
ニツケル合金、コバルト合金、鉄基合金、マンガ
ン基合金などが従来より用いられている。しかし
て、Mn−Sb基合金は高特性磁性膜のスパツタタ
ーゲツト又は蒸着用母合金としての需要が極めて
大きい。
［発明が解決しようとする問題点］
従来より用いられている磁性合金について種々
検討を重ねたところ、酸素、窒素、硫黄、炭素、
その他金属酸化物等の介在物が比較的多量に含ま
れており、得られる薄膜の磁気特性に多大な悪影
響をもたらすことが認められた。
［問題点を解決するための手段］
本発明は上記従来の実情に鑑み、不純物含有量
の少ない高特性磁性薄膜を安定かつ効率的に得る
ことができる蒸着用Mn−Sb基合金を提供するべ
くなくされたものであつて、
Sb35〜75重量％、Al3重量％以下、Ca500ppm
以下、O300ppm以下、N30ppm以下を含有し、
残部が実質的にMnであることを特徴とする蒸着
用Mn−Sb基合金、及び
Sb35〜75重量％、Pt30重量％以下、Al3重量％
以下、Ca500ppm以下、O300ppm以下、N30ppm
以下を含有し、残部が実質的にMnであることを
特徴とする蒸着用Mn−Sb基合金、
を要旨とするものである。
即ち、本発明者は、蒸着用合金の不純物に起因
する問題を解決し、高特性磁性薄膜を得るべく、
鋭意検討を重ねた結果、蒸着用Mn−Sb基合金中
に、特定量のCaとAlとを含有させることにより、
不純物含有量の少ない合金が得られ、しかもCa
とAlとによるゲツタ作用により、蒸着雰囲気中
のガス成分をも低減し、極めて高純度で高特性の
磁性薄膜を得ることができることを身出し、本発
明を完成させた。
なお、Mn基合金については、溶解品が得難
く、従来は、焼結品が殆どであつた。本発明は、
このようなMn基合金について、溶製を容易に行
なえるようにしたものである。
以下、本発明につき詳細に説明する。
なお、本明細書において、「％」は「重量％」
を表すものである。
本発明の蒸着用Mn−Sb基合金は、真空蒸着あ
るいはスパツタリング、イオンプレーテイング等
の蒸着用材料として用いられ、磁性薄膜の製造等
に利用されるものであつて、その組成は、下記の
通りである。
Sb：35〜75％
Mn：残部
Pt：含有せず（第１の発明）又は30％以下（第
２の発明）
Al：３％以下
Ca：500ppm以下
Ｏ：300ppm以下
Ｎ：30ppm
以下に本発明の合金組成の限定理由について説
明する。
本発明の蒸着用Mn−Sb基合金において、Sbは
35〜75％とする。これは、この範囲のSb含有率
にて、極めて高い磁気光学効果（Kerr回転角）
が得られ、高磁気特性の合金となるためであつ
て、好ましいSb含有率は55〜75％、特に65〜70
％とすることにより、著しく高い磁気特性が得ら
れる。
Ptは結晶磁気異方性の向上に作用する。しか
しながら、その含有量が多過ぎると逆に磁気特性
に悪影響を及ぼすことがあるので、本発明におい
てはPtは30％以下、好ましくは20％以下とする。
Alは、合金の溶製を行なう際に、Caと共に合
金の清浄化に作用し、また蒸着雰囲気中にてガス
成分を補捉するゲツタ作用を有する。ただし、
Alはその量があまりに多過ぎ、合金特性に影響
を及ぼす量であつては好ましくなく、このため本
発明においては、前述の如く、Alは３％以下、
当然のことながら、Alは、その量があまりに少
な過ぎると上記清浄化作用及びゲツタ作用による
十分な効果が得られない。本発明においては、
Alは、１〜３％、より好ましくは２〜３％含有
させるのが望ましい。なお、Alは、固溶Alの形
態で合金中に存在することにより、本発明の効果
を奏するものであるので、Alの存在形態は固溶
状態であることが重要である。
Caは前述の如くAlと共に合金の清浄化に作用
し、またゲツタ作用を奏する。Caは、その含有
量があまりに多過ぎると合金特性に影響を及ぼ
し、また、金属間化合物の析出により合金を脆く
することがある。このため、本発明においては
Ca含有量は500ppm以下とする。一方、Ca含有量
は少な過ぎてもCaによる十分な清浄化作用及び
ゲツタ作用が表れない。このようなことから、
Ca含有量は50〜200ppmの範囲とするのが好まし
い。なお、CaはCaOないしCaO−Al2O3の形態で
は本発明の効果は奏し得ないことから、合金中の
Caの存在形態は金属Caであることが重量である。
合金中のＯ、Ｎの量が多いと、蒸着に使用した
際に、蒸着雰囲気の真空度を悪化させたり、また
良好な蒸着が行なえず、高特性の磁性薄膜が得ら
れない。このため、合金中の含有量は300ppm以
下、好ましくは200ppm以下、Ｎ含有量は30ppm
以下、好ましくは10ppm以下とする。
なお、本発明において、Si、Ｐ、Ｓ等の不純物
が合金中に不可避的に含有されるのは、特に問題
とならないが、上述したことと同様の理由から、
本発明において、合金中の他の不純物はできるだ
け少なくするのが良く、例えば、Si含有量は0.1
％以下、Ｐ含有量は200ppm以下、Ｓ含有量は
30ppm以下とするのが好ましい。
このような本発明の蒸着用Mn−Sb基合金は、
例えば、以下に説明する方法に従つて製造するこ
とができる。
即ち、まず、合金中のためのMn、Sb、場合に
よりPt、Alの金属又は合金材料を、内面がCaO
質耐火材で構成された容器中で、真空又はアルゴ
ン等の不活性ガス雰囲気等の非酸化性雰囲気に
て、常法例えば高周波あるいは低周波誘導加熱法
等で加熱して溶解することにより、所望の組成の
合金溶湯を得る。
本発明において、用いられる容器の内面を構成
するCaO質耐火材としては、カルシア（CaO）、
ラルナイト（安定化2CaO・SbO2）、メルウイナ
イト（3CaO・MgO・2SbO2）、アノルサイト
（CaO・Al2O3・2SbO2）ならびにCaOを富化した
ドロマイト等が挙げられるが、特に、電融カルシ
アが好適である。
このようなカルシア質炉材は、そのCaO含有率
が40％以上、特に60％以上のものが好ましい。
CaOは高融点であると共に、高温で極めて安定
であり、溶製にあたり、金属酸化物を生成して溶
湯を不純物により汚染することがなく、高清浄を
溶湯を得ることが可能とされる。
特に、CaO含有量の高いCaO質耐火材で内面が
構成された容器を用いた場合には、脱Ｏ、脱Ｓ、
脱介在物等の精錬作用も奏され、極めて有利であ
る。
しかも、溶湯中にAlが存在するため、溶湯中
の脱Ｏ、脱Ｓ、脱Ｎが行なわれ、また、溶湯中へ
のCaの溶出もおこる。即ち、Alは溶湯中のＯ及
び炉壁のCaOと溶湯中のＳと反応して
CaO＋Ｓ→CaS＋Ｏ
となつて生じたＯと反応して、
2Al＋3O→Al2O3
となり、Al2O3を生じる。また溶湯中のAlは炉壁
のCaOと反応して
2Al＋3CaO→Al2O3＋3Ca（ｇ）
となり、これによつてもAl2O3が生じる。（この
場合、生じたCaは殆ど溶解せずに、ガスとなつ
て系外に抜けるが、ごく一部が合金中に残留し
て、本発明の合金のCa含有量を満足させる。）
Al2O3は次式の如く炉壁のCaOと反応して、
3CaO・Al2O3又は12CaO・7Al2O3の活性な層が
炉壁表面に形成される。
Al2O3＋3CaO→3CaO・Al2O3
7Al2O3＋12CaO→12CaO・7Al2O3
この12CaO・7Al2O3及び3CaO・Al2O3、特に
3CaO・Al2O3は溶湯の脱Ｓ能が高く、脱Ｓが良
好に進行する。
このように、Alにより脱Ｏが、またAlの還元
作用により生じた活性な3CaO・Al2O3、
12CaO・7Al2O3やCaOにより脱Ｓが行なわれる。
また溶湯中のＮは前述のAlとCaOとの反応に
より生じたCa等の蒸発（沸騰）等に伴つて溶湯
中から離脱し、溶湯中のＮ量も低減される。
従つて、内面がCaO質耐火材で構成された容器
中で溶製を行なうことにより、本発明の低Ｏ、低
Ｎ含有量のMn−Sb基合金を容易に得ることがで
きる。
ところで、本発明においては、内面がCaO質耐
火材で構成された容器中にて溶製する際に、Al
を冷却固化後のAl残留量が本発明の範囲、即ち、
Al3％以下となるように添加するのであるが、溶
製に用いる容器の内面を、特に電融カルシアより
なるものとすることにより、Alの添加により溶
湯中へのCaのコンタミを低減し、得られる合金
中のCa含有量を容易に本発明の範囲即ち500ppm
以下とすることができる。
このようにして得られた合金溶湯を、常法に従
つて非酸化性雰囲気下で鋳造する。
この際、鋳造に用いる鋳型の材質としては、
Al2O3、ZrO2、SbO2又はCaO質耐火材等が挙げ
られ、これらのうち、AI2O3、ZrO2、CaO耐火
材、とりわけCaO質耐火材が好適である。
このような方法によれば、Sb35〜75％、場合
によりPt30％以下、Al3％以下、Ca500ppm以下、
O300ppm以下、N30ppm以下を含有し、残部が
実質的にMnである本発明の蒸着用Mn−Sb基合
金を極めて容易に製造することができる。
［作用］
本発明の蒸着用Mn−Sb基合金は、Ｏ、Ｎ含有
量が少ないため、高特性の磁性薄膜を得ることが
できる。
また、本発明の蒸着用Mn−Sb基合金に含有さ
れるAl、Caは、真空蒸着又はスパツタリング等
の蒸着雰囲気にて、
4Al＋3O2→2Al2O3
2Al＋N2→2AlN
2Ca＋O2→2CaO
3Ca＋N2→Ca3N2
のように反応して、雰囲気中のガス成分を低下さ
せる、いわゆるゲツタ作用を奏する。
このため、蒸着時の薄膜形成安定性及び形成速
度を向上させると共に、得られる薄膜は高純度で
磁気特性が大幅に改善され、高特性薄膜を高生産
高率で製造することを可能とする。
［実施例］
以下、実施例について説明する。
実施例 １
第１表に示す組成のMn−Sb基合金を蒸着用材
料として用い、下記仕様のスパツタリング装置に
て、直径10cmのガラス基盤上に薄膜を形成した。
なお、基盤加熱温度は200〜400℃とした。
スパツタリング装置仕様
RFマグネトロンスパツタ装置
(1) ターゲツトサイズ φ4″
(2) 到達圧力 10-7torr
(3) スパツタリングレート 4000Å／min
（基盤固定時）
[Industrial Application Field] The present invention relates to a Mn-Sb-based alloy for vapor deposition, and particularly to a Mn-Sb-based alloy for vapor deposition suitable for manufacturing thin films used as magnetic recording materials. [Prior Art] A magnetic recording material in which a magnetic alloy thin film is formed on a nonmagnetic substrate is well known. Sputtering, vacuum deposition, and ion plating are widely used as methods for producing thin films of magnetic recording materials. In particular, the sputtering method is advantageous in that it is possible to obtain a compositionally uniform thin film while controlling the pressure inside the sputtering device, as long as a target material containing a certain alloying element with a uniform internal composition is obtained. It is. As a ferromagnetic alloy that forms a magnetic alloy thin film,
Nickel alloys, cobalt alloys, iron-based alloys, manganese-based alloys, etc. have been used conventionally. Therefore, Mn--Sb based alloys are in extremely high demand as sputter targets or vapor deposition master alloys for high-performance magnetic films. [Problems to be solved by the invention] After conducting various studies on conventionally used magnetic alloys, we found that oxygen, nitrogen, sulfur, carbon,
It was found that a relatively large amount of other inclusions such as metal oxides were included, and this had a significant adverse effect on the magnetic properties of the resulting thin film. [Means for Solving the Problems] In view of the above-mentioned conventional circumstances, the present invention aims to provide a Mn-Sb-based alloy for deposition, which can stably and efficiently obtain a high-performance magnetic thin film with a low impurity content. Sb35-75% by weight, Al3% by weight or less, Ca500ppm
Contains 300ppm or less of O, 30ppm or less of N,
Mn-Sb based alloy for deposition, characterized in that the balance is substantially Mn, and 35 to 75% by weight of Sb, 30% by weight or less of Pt, and 3% by weight of Al.
Below, Ca500ppm or less, O300ppm or less, N30ppm
A Mn-Sb-based alloy for deposition, characterized in that it contains the following, with the remainder being substantially Mn. That is, the present inventors aimed to solve the problem caused by impurities in the deposition alloy and obtain a high-characteristic magnetic thin film.
As a result of extensive research, we found that by incorporating specific amounts of Ca and Al into the Mn-Sb-based alloy for vapor deposition,
Alloys with low impurity content can be obtained, and Ca
The inventors completed the present invention by discovering that the getter action of Al and Al reduces the gas components in the deposition atmosphere, allowing a magnetic thin film with extremely high purity and high properties to be obtained. Regarding Mn-based alloys, it is difficult to obtain melted products, and conventionally, most of them have been sintered products. The present invention
This Mn-based alloy can be easily melted. Hereinafter, the present invention will be explained in detail. In addition, in this specification, "%" is "weight%"
It represents. The Mn-Sb-based alloy for deposition of the present invention is used as a material for deposition in vacuum deposition, sputtering, ion plating, etc., and is used for manufacturing magnetic thin films, etc., and its composition is as follows. It is. Sb: 35-75% Mn: Balance Pt: None (first invention) or 30% or less (second invention) Al: 3% or less Ca: 500ppm or less O: 300ppm or less N: 30ppm or less of the present invention The reasons for limiting the alloy composition will be explained. In the Mn-Sb-based alloy for vapor deposition of the present invention, Sb is
35-75%. This is due to the extremely high magneto-optical effect (Kerr rotation angle) at this range of Sb content.
The preferred Sb content is 55 to 75%, particularly 65 to 70%.
%, extremely high magnetic properties can be obtained. Pt acts to improve magnetocrystalline anisotropy. However, if its content is too large, it may adversely affect the magnetic properties, so in the present invention, the content of Pt is set to 30% or less, preferably 20% or less. Al works together with Ca to clean the alloy when melting the alloy, and also has a getter action that traps gas components in the deposition atmosphere. however,
It is not preferable that the amount of Al is too large and affects the properties of the alloy. Therefore, in the present invention, as mentioned above, the amount of Al is 3% or less.
Naturally, if the amount of Al is too small, sufficient effects due to the above-mentioned cleaning action and getter action cannot be obtained. In the present invention,
It is desirable to contain Al in an amount of 1 to 3%, more preferably 2 to 3%. Note that since Al exhibits the effects of the present invention by existing in the alloy in the form of solid solution Al, it is important that Al exists in the solid solution state. As mentioned above, Ca works together with Al to clean the alloy and also has a getter action. If the Ca content is too large, it may affect the alloy properties and may also cause the alloy to become brittle due to the precipitation of intermetallic compounds. Therefore, in the present invention,
Ca content shall be 500ppm or less. On the other hand, even if the Ca content is too low, sufficient cleaning and scavenging effects due to Ca will not be exhibited. From such a thing,
The Ca content is preferably in the range of 50 to 200 ppm. Note that since the effects of the present invention cannot be achieved when Ca is in the form of CaO or CaO-Al 2 O 3 , Ca in the alloy is
The weight is that the existing form of Ca is metallic Ca. If the amounts of O and N in the alloy are large, the degree of vacuum in the vapor deposition atmosphere will deteriorate when the alloy is used for vapor deposition, and good vapor deposition will not be possible, making it impossible to obtain a magnetic thin film with high characteristics. Therefore, the content in the alloy is 300ppm or less, preferably 200ppm or less, and the N content is 30ppm.
Below, preferably 10 ppm or less. In the present invention, it is not a particular problem that impurities such as Si, P, and S are unavoidably contained in the alloy, but for the same reason as mentioned above,
In the present invention, it is preferable to reduce other impurities in the alloy as much as possible, for example, the Si content is 0.1
% or less, P content is 200ppm or less, S content is
The content is preferably 30 ppm or less. Such a Mn-Sb-based alloy for vapor deposition of the present invention is
For example, it can be manufactured according to the method described below. That is, first, a metal or alloy material of Mn, Sb, and in some cases Pt or Al for the alloy is used, and the inner surface is made of CaO.
In a container made of high quality refractory material, in a non-oxidizing atmosphere such as vacuum or an inert gas atmosphere such as argon, the desired material is melted by heating using a conventional method such as high frequency or low frequency induction heating. Obtain a molten alloy with a composition of In the present invention, the CaO refractory material constituting the inner surface of the container used is calcia (CaO),
Larnite (stabilized 2CaO・SbO 2 ), merwinite (3CaO・MgO・2SbO 2 ), anorthite (CaO・Al 2 O 3・2SbO 2 ), and CaO-enriched dolomite are included, but in particular, fused calcia is suitable. Such calcia furnace material preferably has a CaO content of 40% or more, particularly 60% or more. CaO has a high melting point and is extremely stable at high temperatures. During melting, CaO does not generate metal oxides and contaminate the molten metal with impurities, making it possible to obtain a highly clean molten metal. In particular, when using a container whose inner surface is made of a CaO-based refractory material with a high CaO content,
It also has a refining effect such as removal of inclusions, which is extremely advantageous. Furthermore, since Al is present in the molten metal, O, S, and N are removed from the molten metal, and Ca is also leached into the molten metal. That is, Al reacts with O in the molten metal, CaO on the furnace wall, and S in the molten metal to form CaO+S→CaS+O, and reacts with the generated O to form 2Al+3O→Al 2 O 3 , producing Al 2 O 3 . . Furthermore, Al in the molten metal reacts with CaO on the furnace wall to form 2Al+3CaO→Al 2 O 3 +3Ca(g), and this also produces Al 2 O 3 . (In this case, the generated Ca hardly dissolves and escapes from the system as a gas, but a small portion remains in the alloy and satisfies the Ca content of the alloy of the present invention.) Al 2 O 3 reacts with CaO on the furnace wall as shown in the following equation,
An active layer of 3CaO.Al 2 O 3 or 12CaO.7Al 2 O 3 is formed on the furnace wall surface. Al 2 O 3 +3CaO→3CaO・Al 2 O 3 7Al 2 O 3 +12CaO→12CaO・7Al 2 O 3This 12CaO・7Al 2 O 3 and 3CaO・Al 2 O 3 , especially
3CaO.Al 2 O 3 has a high ability to remove S from molten metal, and S removal progresses well. In this way, active 3CaO・Al 2 O 3 generated by O removal by Al and the reduction action of Al,
S removal is performed using 12CaO・7Al 2 O 3 and CaO. Further, N in the molten metal is removed from the molten metal due to evaporation (boiling) of Ca, etc. generated by the reaction between Al and CaO as described above, and the amount of N in the molten metal is also reduced. Therefore, by carrying out melting in a container whose inner surface is made of a CaO refractory material, the Mn-Sb-based alloy of the present invention having a low O and N content can be easily obtained. By the way, in the present invention, Al
The amount of Al remaining after cooling and solidifying is within the range of the present invention, that is,
Al is added so that the content is 3% or less, but by making the inner surface of the container used for melting especially made of fused calcia, the addition of Al reduces Ca contamination in the molten metal and increases the yield. The Ca content in the alloy can be easily reduced to the range of the present invention, i.e. 500ppm.
It can be as follows. The molten alloy thus obtained is cast in a non-oxidizing atmosphere according to a conventional method. At this time, the material of the mold used for casting is as follows:
Examples include Al 2 O 3 , ZrO 2 , SbO 2 or CaO refractory materials, and among these, AI 2 O 3 , ZrO 2 , CaO refractory materials, and especially CaO refractory materials are preferred. According to this method, Sb35-75%, Pt30% or less in some cases, Al3% or less, Ca500ppm or less,
The Mn-Sb-based alloy for vapor deposition of the present invention containing 300 ppm or less of O, 30 ppm or less of N, and the balance being substantially Mn can be produced very easily. [Function] Since the Mn-Sb-based alloy for vapor deposition of the present invention has low O and N contents, a magnetic thin film with high characteristics can be obtained. Moreover, Al and Ca contained in the Mn-Sb-based alloy for vapor deposition of the present invention are 4Al+3O 2 →2Al 2 O 3 2Al+N 2 →2AlN 2Ca+O 2 →2CaO 3Ca+N 2 → in a vapor deposition atmosphere such as vacuum evaporation or sputtering . It reacts like Ca 3 N 2 and exhibits a so-called getter effect that lowers gas components in the atmosphere. Therefore, the stability and formation speed of thin film formation during vapor deposition are improved, and the resulting thin film has high purity and greatly improved magnetic properties, making it possible to manufacture high-performance thin films at a high production rate. [Example] Examples will be described below. Example 1 Using a Mn-Sb-based alloy having the composition shown in Table 1 as a deposition material, a thin film was formed on a glass substrate with a diameter of 10 cm using a sputtering apparatus having the following specifications.
Note that the substrate heating temperature was 200 to 400°C. Sputtering equipment specifications RF magnetron sputtering equipment (1) Target size φ4″ (2) Ultimate pressure 10 -7 torr (3) Sputtering rate 4000Å/min (when the base is fixed)
【表】
スパツタ電力、アルゴンガス圧、スパツタ時間
を変えて、各蒸着用材料により形成された薄膜の
膜厚を調べた結果を、それぞれ第１図〜第３図に
示す。
第１図〜第３図より、本発明の蒸着用Mn−Sb
基合金は、膜形成功率が高いことが認められる。
実施例 ２
実施例１で用いたスツパリング装置及び基盤を
用い、第１表のNo.１の蒸着用合金にて、Ar圧又
は基板加熱温度を変えて、それぞれ0.5μｍ厚さの
薄膜を形成して磁気記録材料を製造した。なお、
スパツタ電力は200Wで行なつた。
得られた磁気記録材料の保磁力Hcを調べ、基
盤加熱温度又はAr圧との関係をそれぞれ第４図、
第５図に示す。
第４図及び第５図より、本発明の蒸着用Mn−
Sb基合金によれば、極めて保持率の高い磁気記
録材料が得らえることが認められる。
実施例 ３
実施例２において、No.１及び２の合金材料より
基盤加熱温度400℃、Ar圧６×10-3torrにて得ら
えた磁気記録材料について、その磁気特性を調べ
た結果を第６図に示す。
第６図より、本発明の蒸着用Mn−Sb基合金に
より得られる磁気記録材料はヒステリシス特性に
優れ、角形比が高く、極めて高特性のものである
ことが認められる。
［発明の効果］
以上詳述した通り、本発明の蒸着用Mn−Sb基
合金は、Ｏ、Ｈ含有量が少ない上に、AlとCaに
よるゲツタ作用により、蒸着雰囲気中のガス成分
が大幅に低減される。
このため、蒸着による膜形成安定性及び膜形成
速度が向上されるとともに、得られる薄膜は高純
度で極めて磁気特性に優れたものとなる。
従つて、本発明の蒸着用Mn−Sb基合金によれ
ば、高特性薄膜を高効率で得ることができ、本発
明の蒸着用Mn−Sb基合金は、光磁気記録材料の
薄膜製造用蒸着材料として極めて有用である。[Table] Figures 1 to 3 show the results of examining the thickness of thin films formed with each deposition material while varying the sputtering power, argon gas pressure, and sputtering time. From FIG. 1 to FIG. 3, Mn-Sb for deposition of the present invention
It is observed that the base alloy has a high film formation success rate. Example 2 Using the sputtering device and substrate used in Example 1, thin films with a thickness of 0.5 μm were formed using the vapor deposition alloy No. 1 in Table 1 by varying the Ar pressure or substrate heating temperature. A magnetic recording material was produced. In addition,
The spatuta power was 200W. The coercive force Hc of the obtained magnetic recording material was investigated, and its relationship with substrate heating temperature or Ar pressure is shown in Figure 4 and
It is shown in FIG. From FIG. 4 and FIG. 5, Mn-
It is recognized that magnetic recording materials with extremely high retention rates can be obtained using Sb-based alloys. Example 3 The results of investigating the magnetic properties of the magnetic recording materials obtained in Example 2 from the alloy materials No. 1 and 2 at a base heating temperature of 400°C and an Ar pressure of 6×10 -3 torr are as follows. It is shown in Figure 6. From FIG. 6, it can be seen that the magnetic recording material obtained from the Mn-Sb based alloy for vapor deposition of the present invention has excellent hysteresis characteristics, a high squareness ratio, and extremely high characteristics. [Effects of the Invention] As detailed above, the Mn-Sb-based alloy for vapor deposition of the present invention has low O and H contents, and due to the gettering action of Al and Ca, gas components in the vapor deposition atmosphere are significantly reduced. Reduced. Therefore, the stability and speed of film formation by vapor deposition are improved, and the obtained thin film has high purity and extremely excellent magnetic properties. Therefore, according to the Mn-Sb-based alloy for vapor deposition of the present invention, a thin film with high properties can be obtained with high efficiency, and the Mn-Sb-based alloy for vapor deposition of the present invention can be used for vapor deposition for manufacturing thin films of magneto-optical recording materials. Extremely useful as a material.
第１図〜第３図は実施例１で得られた結果を示
すグラフであつて、それぞれ、スパツタ電圧、ア
ルゴン圧、スパツタ時間と得られる膜厚との関係
を示す。第４図及び第５図は実施例２で得られた
結果を示すグラフであつて、それぞれ、基盤加熱
温度、アルゴン圧と磁気記録材料の保持率との関
係を示す。第６図は実施例３で得られた磁気特性
の測定結果を示すグラフである。
1 to 3 are graphs showing the results obtained in Example 1, and each shows the relationship between sputtering voltage, argon pressure, sputtering time, and the resulting film thickness. FIGS. 4 and 5 are graphs showing the results obtained in Example 2, and show the relationships between substrate heating temperature, argon pressure, and retention rate of the magnetic recording material, respectively. FIG. 6 is a graph showing the measurement results of magnetic properties obtained in Example 3.
Claims (1)
Ca500ppm以下、O300ppm以下、N30ppm以下を
含有し、残部が実質的にMnであることを特徴と
する蒸着用Mn−Sb基合金。 ２ Sb35〜75重量％、Pt30重量％以下、Al3重量
％以下、Ca500ppm以下、O300ppm以下、
N30ppm以下を含有し、残部が実質的にMnであ
ることを特徴とする蒸着用Mn−Sb基合金。[Claims] 1 Sb35 to 75% by weight, Al3% by weight or less,
A Mn-Sb-based alloy for deposition, characterized in that it contains 500 ppm or less of Ca, 300 ppm or less of O, and 30 ppm or less of N, with the remainder being substantially Mn. 2 Sb35-75% by weight, Pt30% by weight or less, Al3% by weight or less, Ca500ppm or less, O300ppm or less,
A Mn-Sb-based alloy for vapor deposition, characterized in that it contains 30 ppm or less of N, with the remainder being substantially Mn.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26710686A JPS63121633A (en) | 1986-11-10 | 1986-11-10 | Mn-sb-based alloy for vapor deposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26710686A JPS63121633A (en) | 1986-11-10 | 1986-11-10 | Mn-sb-based alloy for vapor deposition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63121633A JPS63121633A (en) | 1988-05-25 |
| JPH0364585B2 true JPH0364585B2 (en) | 1991-10-07 |
Family
ID=17440147
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26710686A Granted JPS63121633A (en) | 1986-11-10 | 1986-11-10 | Mn-sb-based alloy for vapor deposition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63121633A (en) |
-
1986
- 1986-11-10 JP JP26710686A patent/JPS63121633A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63121633A (en) | 1988-05-25 |
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