JPS63100149A - Fe-co-base alloy for vapor deposition - Google Patents
Fe-co-base alloy for vapor depositionInfo
- Publication number
- JPS63100149A JPS63100149A JP24362986A JP24362986A JPS63100149A JP S63100149 A JPS63100149 A JP S63100149A JP 24362986 A JP24362986 A JP 24362986A JP 24362986 A JP24362986 A JP 24362986A JP S63100149 A JPS63100149 A JP S63100149A
- Authority
- JP
- Japan
- Prior art keywords
- less
- vapor deposition
- alloy
- thin film
- present
- 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.)
- Granted
Links
- 239000000956 alloy Substances 0.000 title claims abstract description 66
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 64
- 238000007740 vapor deposition Methods 0.000 title claims abstract description 38
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 11
- 229910017061 Fe Co Inorganic materials 0.000 claims description 14
- 239000010409 thin film Substances 0.000 abstract description 28
- 230000005291 magnetic effect Effects 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910052759 nickel Inorganic materials 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 238000005247 gettering Methods 0.000 abstract description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 22
- 239000000292 calcium oxide Substances 0.000 description 22
- 235000012255 calcium oxide Nutrition 0.000 description 22
- 230000000694 effects Effects 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 15
- 238000004544 sputter deposition Methods 0.000 description 15
- 239000002184 metal Substances 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000000151 deposition Methods 0.000 description 10
- 230000008021 deposition Effects 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 239000011819 refractory material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910017112 Fe—C Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910001004 magnetic alloy Inorganic materials 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 150000002500 ions Chemical class 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
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000007738 vacuum evaporation 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
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 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
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052737 gold 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
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Thin Magnetic Films (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
[a業上の利用分野]
本発明は蒸着用Fe−Co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Fe−
Co基合金に関する。Detailed Description of the Invention [Field of Application in Industry A] The present invention relates to a Fe-Co-based alloy for deposition, and in particular to a Fe-Co-based alloy for deposition, which is suitable for manufacturing thin films used as magnetic recording materials.
It relates to a Co-based alloy.
[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。[Prior Art] A magnetic recording material in which a magnetic alloy thin film is formed on a nonmagnetic substrate is well known.
この磁気記録材料の薄膜を製造する方法としては、スパ
ッタリングや真空蒸着、イオンブレーティング等の蒸着
法が広く用いられている。Vapor deposition methods such as sputtering, vacuum evaporation, and ion blating are widely used as methods for producing thin films of magnetic recording materials.
特にスパッタリング法は、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、スパッ
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。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. be.
磁性合金薄膜を形成する強磁性合金としては、ニッケル
合金、コバルト合金、鉄基合金などが従来より用いられ
ている。Conventionally, nickel alloys, cobalt alloys, iron-based alloys, and the like have been used as ferromagnetic alloys for forming magnetic alloy thin films.
ところで、近年、特に光磁気ディスク材としてR,E−
T、M型の合金が注目を集めている。By the way, in recent years, R, E-
T and M type alloys are attracting attention.
ここでR,Eは希土類元素で具体的にはTb。Here, R and E are rare earth elements, specifically Tb.
Gd% Dy5Nd、Hoなど、また、T、Mは遷移金
属元素でFe%Co%Niが代表的なものとして知られ
ている。Gd% Dy5Nd, Ho, etc., and T and M are transition metal elements, and Fe%Co%Ni is known as a typical example.
これらのR,E−T、M型合金の薄膜をスパッタ又は真
空蒸着により得る場合、R,E−T、M系合金の蒸着源
を用いる他、R,E系とT、M系との別々の蒸着源を用
いて蒸着(又はスパッタ)を行ない、最終的に目的のR
,E−T、M系合金組成の膜を得る方法がある(多元ス
パッタ)。When obtaining thin films of these R, E-T, and M type alloys by sputtering or vacuum evaporation, in addition to using a deposition source for the R, E-T, and M type alloys, separate Vapor deposition (or sputtering) is performed using a vapor deposition source, and finally the desired R
, ET, and M-based alloy compositions (multiple sputtering).
このような多元スパッタに用いるT、M合金ととしては
、Fe、Co% Fe−Co系が知られており、特に不
純物含有量の少ない均質な合金であることが要求されて
いる。As the T and M alloys used in such multi-component sputtering, Fe and Co% Fe-Co systems are known, and in particular, a homogeneous alloy with a low impurity content is required.
[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。[Problems to be solved by the invention] After conducting various studies on conventionally used magnetic alloys, we found that they contain relatively large amounts of inclusions such as oxygen, nitrogen, sulfur, carbon, and other metal oxides. It has been recognized that this has a significant adverse effect on the magnetic properties of the resulting thin film.
[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Fe−Co基合金を提供するべくなされたものであ
って、
Co5〜95重量%、Au1li量%以下、Ca及び/
又はMMg300pp以下、030ppmm以下、NN
30pp以下を含有し、残部が実質的にFeであること
を特徴とする蒸着用Fe−C。[Means for Solving the Problems] In view of the above-mentioned conventional situation, the present invention aims to provide a Fe-Co-based alloy for deposition, which can stably and efficiently obtain a high-characteristic magnetic thin film with a low impurity content. Co5-95% by weight, Au1li% or less, Ca and/or
or MMg 300pp or less, 030ppmm or less, NN
Fe-C for deposition, characterized in that it contains 30 pp or less, and the remainder is substantially Fe.
基合金、
005〜95重量%、A11重量%以下、Ti1重量%
以下、Ca及び/又はMMg300pp以下、030p
pm以下、NN30pp以下を含有し、残部が実質的に
Feであることを特徴とする蒸着用Fe−Co基合金、
005〜95重量%、Ni及び/又はCr20重量%以
下、Al21重量%以下、Ca及び/又はMMg300
pp以下、030ppm以下、NN30pp以下を含有
し、残部が実質的にFeであることを特徴とする蒸着用
Fa−Co基合金、及び
005〜95重量%、Ni及び/又はCr20重量%以
下、Al1重量%以下、Ti1重量%以下、Ca及び/
又はMMg300pP以下、030ppm以下、NN3
0pp以下を含有し、残部が実質的にFeであることを
特徴とするFe−Co基合金、
を要旨とするものである。Base alloy, 005-95% by weight, A11% by weight or less, Ti 1% by weight
Below, Ca and/or MMg 300pp or less, 030p
A Fe-Co-based alloy for vapor deposition, characterized in that it contains 0.05 to 95% by weight, 20% by weight or less of Ni and/or Cr, 21% by weight or less of Al, the balance being substantially Fe. Ca and/or MMg300
Fa-Co based alloy for vapor deposition, characterized in that it contains NN30pp or less, NN30pp or less, and the balance is substantially Fe, and 005 to 95% by weight, Ni and/or Cr20% by weight or less, Al1 % by weight or less, Ti 1% by weight or less, Ca and/or
or MMg 300pP or less, 030ppm or less, NN3
An Fe--Co based alloy containing 0 pp or less and the remainder being substantially Fe.
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Fe−Co基合金中に、特定量のCa及
び/又はMgと、Au2あるいはAu及びTi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及び/又はMgとAu2及び/又はTiと
によるゲッタ作用により、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
できることを見出し、本発明を完成させた。That is, as a result of extensive studies in order to solve the problem caused by impurities in the deposition alloy and obtain a high-characteristic magnetic thin film, the present inventor has found that a specific amount of Ca and By containing Mg and Au2 or Au and Ti, an alloy with low impurity content can be obtained, and due to the getter action of Ca and/or Mg and Au2 and/or Ti, gas in the deposition atmosphere can be obtained. The present invention was completed by discovering that it is possible to obtain a magnetic thin film with extremely high purity and high characteristics by reducing the amount of components.
以下、本発明につき詳細に説明する。Hereinafter, the present invention will be explained in detail.
なお、本明細書において、1%」は「重量%」を表すも
のである。In addition, in this specification, "1%" represents "weight%."
本発明の蒸着用Fe−Co基合金は、真空蒸着あるいは
スパッタリング、イオンブレーティ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
あって、その組成は、下記の通りである。The Fe-Co-based alloy for vapor deposition of the present invention is used as a material for vapor deposition in vacuum vapor deposition, sputtering, ion blating, etc., and is used for manufacturing magnetic thin films, etc., and its composition is as follows. It is.
Co:5〜95%
Ni及び/又はCr:
含有せず(第1の発明及び第2の発
明)又は20%以下(第3の発明及び
第4の発明)
Fe:残部
Al171%以下
Ti:含有せず(第1の発明及び第3の発明)又は1%
以下(第2の発明及び第
4の発明)
Ca及び/又はMg : 300ppm以下0 :3
0ppm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。Co: 5 to 95% Ni and/or Cr: Not contained (first invention and second invention) or 20% or less (third invention and fourth invention) Fe: Balance Al 171% or less Ti: Contained None (first invention and third invention) or 1%
The following (second invention and fourth invention) Ca and/or Mg: 300 ppm or less 0:3
0 ppm or less N: 30 ppm The reason for limiting the alloy composition of the present invention will be explained below.
本発明の蒸着用Fe−Co基合金において、COは5〜
95%とする。これは、この範囲のCo含有率にて、極
めて高い保磁率やヒステリシス特性の向上効果が得られ
るためであって、好ましいCo含有率は5〜70%、特
に10〜60%とすることにより、著しく良好な薄膜が
得られる。In the Fe-Co-based alloy for vapor deposition of the present invention, CO is 5 to
It shall be 95%. This is because an extremely high coercivity and improvement in hysteresis characteristics can be obtained with a Co content in this range, and the preferred Co content is 5 to 70%, particularly 10 to 60%. A very good thin film is obtained.
Ni及び/又はCrは磁気特性の向上及び耐食性の向上
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Cr20%以下、特に15%以下とする。Ni and/or Cr work to improve magnetic properties and corrosion resistance. However, if the Cr content is too large, it may adversely affect the magnetic properties, so in the present invention, the Cr content is set to 20% or less, particularly 15% or less.
An及びTiは、合金の溶製を行なう際に、Ca、Mg
と共に合金の清浄化に作用し、また蒸着雰囲気中にてガ
ス成分を捕捉するゲッタ作用を有する。ただし、Al1
、Tiはその量があまりに多過ぎ、合金特性に影響を及
ぼす量であっては好ましくなく、このため本発明におい
ては、各々1%以下とする。当然のことながら、Al1
、Tiは、その量があまりに少な過ぎると上記清浄化作
用及びゲッタ作用による十分な効果が得られない0本発
明においては、Al20,005〜0.5%、あるいは
、AIo、005〜0.5%及びTi0.5%以下、よ
り好ましくはAl20,01〜0,2、あるいは、Aj
!0.01〜0.2%及びTi0.2%以下とするのが
望ましい。なお、A1又はTiは、固溶AIL又は固溶
Tiの形態で合金中に存在することにより、本発明の効
果を奥するものであるので、Al1又はTiの存在形態
は固溶状態であることが重要である。An and Ti are mixed with Ca and Mg when melting the alloy.
It also acts to clean the alloy and has a getter effect to trap gas components in the deposition atmosphere. However, Al1
, Ti are in too large an amount, and it is not preferable that the amount affects the alloy properties. Therefore, in the present invention, each of them is set to 1% or less. Naturally, Al1
, Ti, if the amount thereof is too small, sufficient effects of the above-mentioned cleaning action and getter action cannot be obtained. % and Ti0.5% or less, more preferably Al20.01-0.2, or Aj
! It is desirable that Ti be 0.01 to 0.2% and Ti be 0.2% or less. Note that the effect of the present invention is enhanced by the presence of A1 or Ti in the alloy in the form of solid solution AIL or solid solution Ti, so the existence form of Al1 or Ti should be in the solid solution state. is important.
Ca、Mgは前述の如<AfL及び/又はTiと共に合
金の清浄化に作用し、またゲッタ作用を臭する。Ca及
びMg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。As mentioned above, Ca and Mg work together with AfL and/or Ti to clean the alloy, and also provide getter action. If the content of Ca and Mg is too large, it may affect the properties of the alloy and may also cause the alloy to become brittle due to the precipitation of intermetallic compounds.
このため、本発明においてはCa及び/又はMgの含有
量は300ppm以下とする。一方、Ca及び/又はM
gの含有量は少な過ぎてもCa。Therefore, in the present invention, the content of Ca and/or Mg is set to 300 ppm or less. On the other hand, Ca and/or M
Even if the content of g is too low, it still contains Ca.
Mgによる十分な清浄化作用及びゲッタ作用が現れない
、このようなことから、Ca、Mg含有量は、各々、5
〜1100ppの範囲、好ましくは各々10〜50pp
mの範囲とするのが好ましい、なお、CaはCaOない
しCa0−AJI!203の形態では本発明の効果は奏
し得す、同様に、MgはMgOの形態では本発明の効果
を臭し得ないことから、合金中のCa%Mgの存在形態
は金属Ca、金属Mgであることが重要である。Because Mg does not exhibit sufficient cleaning and gettering effects, the Ca and Mg contents are each 5
~1100pp, preferably 10-50pp each
It is preferable that Ca is in the range of m, and Ca is CaO to Ca0-AJI! The effect of the present invention can be achieved in the form of 203. Similarly, the effect of the present invention cannot be achieved when Mg is in the form of MgO, so the existence form of Ca%Mg in the alloy is It is important that there be.
合金中の0、Nの量が多いと、蒸着に使用した際に、蒸
着雰囲気の真装置を悪化させたり、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0含有量は30ppm以下、好ましくは20pp
m以下、N含有量は30ppm以下、好ましくは20p
pm以下とする。If the amount of 0 and N in the alloy is large, when used for vapor deposition, the quality of the vapor deposition atmosphere will deteriorate, or good vapor deposition will not be possible, making it impossible to obtain a magnetic thin film with high characteristics. Therefore, the 0 content in the alloy is less than 30 ppm, preferably 20 ppm.
m or less, N content is 30 ppm or less, preferably 20 p
pm or less.
なお、本発明において、Si%Mn、P%S等の不純物
が合金中に不可避的に含有されるのは、特に問題とはな
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、Mn含有量
は0.05%以下、P含有量は50ppm以下、S含有
量は20ppm以下とするのが好ましい。In the present invention, it is not a particular problem that impurities such as Si%Mn and P%S are unavoidably contained in the alloy. It is better to reduce other impurities in it as much as possible, for example, the Si content is 0.1% or less, the Mn content is 0.05% or less, the P content is 50ppm or less, and the S content is 20ppm or less. is preferable.
このような本発明の蒸着用Fe−Co基合金は、例えば
、以下に説明する方法に従って製造することができる。Such a Fe-Co-based alloy for vapor deposition of the present invention can be manufactured, for example, according to the method described below.
即ち、まず、合金化のためのCO1場合によりNi及び
/又はCr%Fe、Al1、場合によりTiの金属又は
合金材料を、内面がCaO貿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話導加
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。That is, first, a metal or alloy material of CO1, optionally Ni and/or Cr%Fe, Al1, optionally Ti for alloying is placed in a container whose inner surface is made of a CaO refractory material under vacuum or argon, etc. A molten alloy having a desired composition is obtained by heating and melting in a non-oxidizing atmosphere such as an inert gas atmosphere using a conventional method such as a high frequency or low frequency induction heating method.
本発明において、用いられる容器の内面を構成するCa
O質耐火材としては、カルシア(Cab)、ラルナイト
(安定化2CaO−3iO2) % メルウィナイト(
3CaO・Mg0・2 S iO2) x アノルサイ
ト(CaO−A110g ”2SiO2)ならびにCa
O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。In the present invention, Ca constituting the inner surface of the container used
Examples of O-grade refractory materials include calcia (Cab), larnite (stabilized 2CaO-3iO2), % melwinite (
3CaO・Mg0・2SiO2) x Anorsite (CaO-A110g “2SiO2) and Ca
Examples include O-enriched dolomite, and fused calcia is particularly preferred.
このようなカルシア貿炉材は、そのCaO含有率が40
%以上、特に60%以上のものが好ましい。Such calcia trading furnace material has a CaO content of 40
% or more, especially 60% or more is preferable.
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、高清浄な溶湯を得ることが可
能とされる。CaO has a high melting point and is extremely stable at high temperatures, making it possible to obtain a highly clean molten metal without producing metal oxides and contaminating the molten metal with impurities during melting.
特に、CaO含有量の高いCaO’Jj耐火材で内面が
構成された容器を用いた場合には、脱01脱S、脱介在
物等の精錬作用も奏され、極めて有利である。In particular, when a container whose inner surface is made of a CaO'Jj refractory material with a high CaO content is used, refining effects such as removal of O1, S and inclusions are also achieved, which is extremely advantageous.
しかも、溶湯中にAJZあるいはAIl及びTiが存在
するため、溶湯中の脱01脱Sが行なわれ、これに伴っ
て脱Nも起こる。また、炉壁材のCaOとAJZとの反
応により溶湯中へのCaの溶出もおこる。即ち、Al1
は溶湯中の0及び炉壁のCaOと溶湯中のSと反応して
CaO+5−Ca5+0
となって生じた0と反応して、
2Al+3O−AIl20s
となり、A旦203を生じる。また溶湯中のAl1は炉
壁のCaOと反応して
2Afl+3CaO=Aft20g +3Ca (g)
となり、これによってもAfa 03が生じる。Moreover, since AJZ or AIl and Ti are present in the molten metal, O1 and S removal in the molten metal is carried out, and along with this, N removal also occurs. Furthermore, Ca is leached into the molten metal due to the reaction between CaO in the furnace wall material and AJZ. That is, Al1
reacts with 0 in the molten metal, CaO on the furnace wall, and S in the molten metal to form CaO+5-Ca5+0, which reacts with the resulting 0 to form 2Al+3O-AIl20s, producing Adan 203. Also, Al1 in the molten metal reacts with CaO on the furnace wall, resulting in 2Afl+3CaO=Aft20g +3Ca (g)
This also results in Afa 03.
(この場合、生じたCaは、ガスとなって系外に抜ける
が、一部が合金中に残留して、本発明の合金のCa含有
量を溝足させる。)
AfL20sは次式の如く炉壁のCaOと反応して、3
CaO・A1203又は12Cao・フAf1wO3の
活性な層が炉壁表面に形成される。(In this case, the generated Ca becomes a gas and escapes from the system, but a portion remains in the alloy and adds to the Ca content of the alloy of the present invention.) AfL20s is a furnace as shown in the following formula. Reacts with CaO on the wall, 3
An active layer of CaO.A1203 or 12Cao.AflwO3 is formed on the furnace wall surface.
A1120g +3CaO−3CaO* A120g7
Alz Os +12CaO=1
2CaO−フAJ!203
この12CaO・フAj!a Os Btび3CaO・
AIl203 、特に3CaO・AlaOsは溶湯の脱
S能が高く、脱Sが良好に進行する。A1120g +3CaO-3CaO* A120g7
Alz Os +12CaO=1 2CaO−F AJ! 203 This 12CaO・fuAj! a Os Btbi3CaO・
Al1203, especially 3CaO.AlaOs, has a high ability to remove S from the molten metal, and S removal progresses well.
このように、Aftにより脱0が、またAIlの還元作
用により生じた活性な3CaO・AfzOs、12Ca
O@ 7Al20sやCaOにより脱Sが行なわれる。In this way, the active 3CaO・AfzOs and 12Ca generated by de0 by Aft and the reducing action of AIl are
S removal is performed by O@7Al20s and CaO.
また、耐火材がCaO−MgO系の容器を用いて溶製を
行なった場合、Caと共にMgの溶出も見られ、溶湯中
に金属態Mgが残留し、Caと同様に蒸着時にゲッタ作
用を臭し、その効果を補完し、更に強力なものとする。In addition, when the refractory material is melted using a CaO-MgO-based container, Mg is also eluted along with Ca, and metallic Mg remains in the molten metal, causing a getter effect during vapor deposition as well as Ca. It complements that effect and makes it even more powerful.
即ち、炉壁のMgOは
3Mg0+CaO+2AJ!−=
CaO@ Al2 20s +3Mg (g)と
なり、生じたMgの一部が合金中に残留する。In other words, the MgO on the furnace wall is 3Mg0+CaO+2AJ! -=CaO@Al2 20s +3Mg (g), and a part of the generated Mg remains in the alloy.
また溶湯中のNは前述のAfLとCaOとの反応により
生じたCa等の蒸発(沸騰)等に伴って溶湯中から離脱
し、溶湯中のN量も低減される。Further, N in the molten metal is removed from the molten metal due to evaporation (boiling) of Ca etc. generated by the above-mentioned reaction between AfL and CaO, and the amount of N in the molten metal is also reduced.
Tiが加わった場合、Al1の作用を補完し、更にAJ
Zと同様の作用により脱0、脱S1脱Nを行なう。When Ti is added, it complements the action of Al1 and further increases AJ.
De-0, de-S1 de-N is performed by the same action as Z.
従って、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0、低N含有量のF
e−Co基合金を容易に得ることができる。Therefore, by carrying out melting in a container whose inner surface is made of CaO-based refractory material, the low zero and low N content F of the present invention can be produced.
An e-Co based alloy can be easily obtained.
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、AnあるいはAf
L及びTiを冷却固化後のAl2あるいはAl2及びT
i残留量が本発明の範囲、即ち、AJZI%以下あるい
はAj21%以下及びTi1%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CaO
及びMgO(MgO含有率60〜15%)のカルシア系
耐火物よりなるものとすることにより、Al1あるいは
Afl及びTiの添加により、溶湯中へCaだけでなく
Mgの溶出も認められ、得られる合金中のCa、Mg含
有量を容易に本発明の範囲即ち300ppm以下とする
ことができる。By the way, in the present invention, when melting is performed in a container whose inner surface is made of CaO-based refractory material, An or Af
Al2 or Al2 and T after cooling and solidifying L and Ti
CaO is added so that the residual amount of i is within the range of the present invention, that is, AJZI% or less, Aj is 21% or less, and Ti is 1% or less.
and MgO (MgO content 60-15%), by adding Al1 or Afl and Ti, not only Ca but also Mg is leached into the molten metal, and the resulting alloy The Ca and Mg contents can be easily controlled within the range of the present invention, that is, 300 ppm or less.
このようにして得られた合金溶湯を、常法に従って非酸
化性雰囲気下で鋳造する。The molten alloy thus obtained is cast in a non-oxidizing atmosphere according to a conventional method.
このような方法によれば、Co5〜95%、場。According to such a method, Co5-95%, field.
合によりNi及び/又はCr20%以下、Al11%以
下、場合によりTi1%以下、Ca及び/又はMMg3
00pp以下、030ppm以下、NN30ppm以下
を含有し、残部が実質的にFeである本発明の蒸着用F
e−Co基合金を極めて容易に製造することができる。Depending on the case, Ni and/or Cr 20% or less, Al 11% or less, Ti 1% or less, Ca and/or MMg3
The F for vapor deposition of the present invention contains 00ppm or less, 030ppm or less, NN30ppm or less, and the balance is substantially Fe.
e-Co-based alloys can be produced very easily.
[作用]
本発明の蒸着用Fe−Co基合金は、0、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。[Function] Since the Fe-Co-based alloy for vapor deposition of the present invention has a low content of 0 and N, a magnetic thin film with high characteristics can be obtained.
また、本発明の蒸着用Fe−Co基合金に含有されるA
fL及びTi、Ca5Mgは、真空蒸着又はスパッタリ
ング等の蒸着雰囲気中にて、4 A J! + 302
−2 A It a O52Al+N2 → 2A
i N2
Ca + 0 2 −* 2 Ca 03
Ca+N 2−+Cas N2の
ように反応して、雰囲気中のガス成分を低下させる、い
わゆるゲッタ作用を奏する。Further, A contained in the Fe-Co-based alloy for vapor deposition of the present invention
fL, Ti, and Ca5Mg are 4 A J! in a vapor deposition atmosphere such as vacuum vapor deposition or sputtering. +302
-2 A It a O52Al+N2 → 2A
i N2 Ca + 0 2 −* 2 Ca 03
It reacts like Ca+N 2-+Cas N2 and exhibits a so-called getter effect that lowers the gas component in the atmosphere.
Ti%Mgについても同様にそれぞれAl1、Caの作
用を下式のように補完して良好なゲッタ作用を奏する。Similarly, Ti%Mg also complements the effects of Al1 and Ca, respectively, as shown in the following formula, and exhibits a good getter effect.
T i +02→TiO2
Ti+N2→TiN2
2Mg+02→2Mg0
3Mg0+N2→Mgs N2
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効率で製造することを
可能とする。T i +02→TiO2 Ti+N2→TiN2 2Mg+02→2Mg0 3Mg0+N2→Mgs N2 Therefore, the thin film formation stability and formation speed during vapor deposition are improved, and the resulting thin film has high purity and greatly improved magnetic properties, resulting in high properties. It makes it possible to manufacture thin films with high production efficiency.
本発明の蒸着用Fe−Co基合金は、特に多元スパッタ
用蒸着源として、R,E系蒸着源の酸化、消耗を低減す
る作用を奏し、極めて有用である。The Fe--Co based alloy for vapor deposition of the present invention is extremely useful, particularly as a vapor deposition source for multi-component sputtering, since it has the effect of reducing oxidation and consumption of R, E-based vapor deposition sources.
[実施例] 以下、実施例について説明する。[Example] Examples will be described below.
実施例1
第1表に示す組成のFe−Co基合金と・・・・・・合
金とを多元スパッタ用材料として用い、下記仕様のスパ
ッタリング装置にて、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150℃とした。Example 1 A thin film was formed on a glass substrate with a diameter of 10 cm using a sputtering apparatus with the following specifications using an Fe-Co-based alloy having the composition shown in Table 1 and an alloy as multi-component sputtering materials. did. Note that the substrate heating temperature was 150°C.
スパッタリング装置土様
マ、グネトロンタイプ高周波スパッタリング装置最大出
カニIKW
到達真空度: 10 ”’torr
ターゲット寸法:100a+m(φ)x3−mm(t)
第1表(Ca、O,Nはppm、mt%)アルゴンガス
圧、スパッタ時間を変えて、各蒸着用材料により形成さ
れた薄膜の膜厚及び膜厚のばらつきを調べた結果を、そ
れぞれ第2表、第3表に示す。Sputtering equipment Tsuchisama, Gnetron type high frequency sputtering equipment Maximum output IKW Ultimate vacuum: 10”'torr Target size: 100a+m (φ) x 3-mm (t)
Table 1 (Ca, O, N: ppm, mt%) The results of examining the film thickness and film thickness variation of thin films formed with each deposition material by changing the argon gas pressure and sputtering time are shown in Table 1. It is shown in Table 2 and Table 3.
第2表、第3表より、本発明の蒸着用Fa−CO基合金
は、膜形成効率が高いことが詔められる。From Tables 2 and 3, it can be said that the Fa-CO based alloy for vapor deposition of the present invention has high film forming efficiency.
第 2 表
* 1部剥離
第3表
実施例2
第1表の動、1〜8の蒸着用合金を用いて、電子ビーム
加熱蒸着を行い、それぞれ1μm厚さの薄膜を形成した
0本蒸着において10−”mmHg下で歯、1〜No、
4の合金の電子ビーム蒸着において、予熱をせずにビ
ームを当てても真空度の変化は殆ど認められず、また突
沸などの現象も認められなかった。Table 2 * 1 Part Peeling Table 3 Example 2 Electron beam heating evaporation was performed using the evaporation alloys 1 to 8 in Table 1 to form a thin film with a thickness of 1 μm. Teeth under 10-”mmHg, 1 to No.
In electron beam evaporation of alloy No. 4, almost no change in the degree of vacuum was observed even when the beam was applied without preheating, and no phenomena such as bumping were observed.
しかしながら比較例5〜Bの合金の場合、電子ビームを
当てた瞬間に真空度は大きく低下すると共に、突沸現象
をおこし湯が一部飛散した。However, in the case of the alloys of Comparative Examples 5 to B, the degree of vacuum significantly decreased at the moment of exposure to the electron beam, and a bumping phenomenon occurred, causing some of the hot water to scatter.
生成した膜についてもその平滑性、膜厚分布などにおい
て合金動、1〜No、 4の場合と勤、5〜歯、8の場
合では大きな差が認められ、明らかに動、1〜No、
4の合金の方が優れていた。Regarding the formed film, there was a large difference in its smoothness, film thickness distribution, etc. between the case of alloy movement, 1 to No. 4, and the case of hardness, 5 to tooth, 8, and it was clearly seen that
Alloy No. 4 was superior.
実施例3
実施例2において、歯、2及び6の合金材料及びGd−
Tb合合材材料2元蒸着を行い、1μm厚さの薄膜を得
た。このようにして得られた磁気記録薄膜について、そ
の磁気特性及び/N比を調べた結果を第4表に示す。Example 3 In Example 2, teeth, alloy materials 2 and 6 and Gd-
A thin film with a thickness of 1 μm was obtained by performing binary evaporation of the Tb composite material. Table 4 shows the results of examining the magnetic properties and /N ratio of the magnetic recording thin film thus obtained.
第4表
第4表より、本発明の蒸着用Fe−Co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。Table 4 From Table 4, it is recognized that the magnetic recording material obtained from the Fe--Co based alloy for vapor deposition of the present invention has excellent hysteresis characteristics, a high squareness ratio, and extremely high characteristics.
[発明の効果] 以上詳述した通り、本発明の蒸着用Fe−C。[Effect of the invention] As detailed above, Fe-C for vapor deposition of the present invention.
基合金は、0、N含有量が少ない上に、AIL、あるい
はAI!及びTiとCa%Mgによるゲッタ作用により
、蒸着雰囲気中のガス成分が大幅に低減される。The base alloy has a low 0, N content, and is AIL or AI! Also, due to the getter action of Ti and Ca%Mg, gas components in the deposition atmosphere are significantly reduced.
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。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.
従って、本発明の蒸着用Fe−C,o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
Fe−Co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。Therefore, according to the Fe-C, o-based alloy for vapor deposition of the present invention,
High-performance thin films can be obtained with high efficiency, and the Fe--Co-based alloy for vapor deposition of the present invention is extremely useful as a vapor deposition material for producing thin films of magneto-optical recording materials.
Claims (4)
び/又はMg300ppm以下、O30ppm以下、N
30ppm以下を含有し、残部が実質的にFeであるこ
とを特徴とする蒸着用Fe−Co基合金。(1) Co5 to 95% by weight, Al 1% by weight or less, Ca and/or Mg 300ppm or less, O 30ppm or less, N
A Fe-Co-based alloy for vapor deposition, characterized in that it contains 30 ppm or less, and the remainder is substantially Fe.
重量%以下、Ca及び/又はMg300ppm以下、O
30ppm以下、N30ppm以下を含有し、残部が実
質的にFeであることを特徴とする蒸着用Fe−Co基
合金。(2) Co5 to 95% by weight, Al 1% by weight or less, Ti1
Weight% or less, Ca and/or Mg 300ppm or less, O
30 ppm or less, N30 ppm or less, and the balance is substantially Fe.
量%以下、Al1重量%以下、Ca及び/又はMg30
0ppm以下、O30ppm以下、N30ppm以下を
含有し、残部が実質的にFeであることを特徴とする蒸
着用Fe−Co基合金。(3) Co5 to 95% by weight, Ni and/or Cr 20% by weight or less, Al 1% by weight or less, Ca and/or Mg30
An Fe-Co-based alloy for vapor deposition, characterized in that it contains 0 ppm or less, O 30 ppm or less, N 30 ppm or less, and the balance is substantially Fe.
量%以下、Al1重量%以下、Ti1重量%以下、Ca
及び/又はMg300ppm以下、O30ppm以下、
N30ppm以下を含有し、残部が実質的にFeである
ことを特徴とする蒸着用Fe−Co基合金。(4) Co5 to 95% by weight, Ni and/or Cr 20% by weight or less, Al 1% by weight or less, Ti 1% by weight or less, Ca
and/or Mg 300ppm or less, O 30ppm or less,
A Fe-Co-based alloy for vapor deposition, characterized in that it contains 30 ppm or less of N, and the remainder is substantially Fe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24362986A JPS63100149A (en) | 1986-10-14 | 1986-10-14 | Fe-co-base alloy for vapor deposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24362986A JPS63100149A (en) | 1986-10-14 | 1986-10-14 | Fe-co-base alloy for vapor deposition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63100149A true JPS63100149A (en) | 1988-05-02 |
| JPH0430451B2 JPH0430451B2 (en) | 1992-05-21 |
Family
ID=17106665
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24362986A Granted JPS63100149A (en) | 1986-10-14 | 1986-10-14 | Fe-co-base alloy for vapor deposition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63100149A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10116749A (en) * | 1996-10-08 | 1998-05-06 | Sony Corp | Method for producing magnetic material for metal thin film magnetic recording medium and metal thin film magnetic recording medium |
| KR100494610B1 (en) * | 1996-02-28 | 2005-09-08 | 미쓰비시 마테리알 가부시키가이샤 | High-Density Sputtering Target for Forming High-Dielectric Films |
| JP2009167529A (en) * | 2009-01-22 | 2009-07-30 | Sanyo Special Steel Co Ltd | Soft magnetic target material |
| JP2019534562A (en) * | 2016-10-27 | 2019-11-28 | ザ ボード オブ トラスティーズ オブ ザ ユニヴァーシティ オブ アラバマ | Fe-Al alloy magnetic thin film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60228637A (en) * | 1984-04-25 | 1985-11-13 | Toshiba Corp | Co alloy for magnetic recording medium |
-
1986
- 1986-10-14 JP JP24362986A patent/JPS63100149A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60228637A (en) * | 1984-04-25 | 1985-11-13 | Toshiba Corp | Co alloy for magnetic recording medium |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100494610B1 (en) * | 1996-02-28 | 2005-09-08 | 미쓰비시 마테리알 가부시키가이샤 | High-Density Sputtering Target for Forming High-Dielectric Films |
| JPH10116749A (en) * | 1996-10-08 | 1998-05-06 | Sony Corp | Method for producing magnetic material for metal thin film magnetic recording medium and metal thin film magnetic recording medium |
| JP2009167529A (en) * | 2009-01-22 | 2009-07-30 | Sanyo Special Steel Co Ltd | Soft magnetic target material |
| JP2019534562A (en) * | 2016-10-27 | 2019-11-28 | ザ ボード オブ トラスティーズ オブ ザ ユニヴァーシティ オブ アラバマ | Fe-Al alloy magnetic thin film |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0430451B2 (en) | 1992-05-21 |
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