JPH0371420A - Perpendicular magnetic recording medium and its production - Google Patents
Perpendicular magnetic recording medium and its productionInfo
- Publication number
- JPH0371420A JPH0371420A JP20813089A JP20813089A JPH0371420A JP H0371420 A JPH0371420 A JP H0371420A JP 20813089 A JP20813089 A JP 20813089A JP 20813089 A JP20813089 A JP 20813089A JP H0371420 A JPH0371420 A JP H0371420A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- fen
- thin film
- magnetic
- perpendicular magnetic
- 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
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 82
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 239000010409 thin film Substances 0.000 claims abstract description 39
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 229910001337 iron nitride Inorganic materials 0.000 claims abstract description 14
- 230000005298 paramagnetic effect Effects 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 229910052742 iron Inorganic materials 0.000 claims description 9
- -1 nitrogen ions Chemical class 0.000 claims description 8
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims description 2
- 239000012790 adhesive layer Substances 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 23
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 7
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 7
- 229910000705 Fe2N Inorganic materials 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 5
- 229910000727 Fe4N Inorganic materials 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 3
- 238000007885 magnetic separation Methods 0.000 abstract description 3
- 238000005191 phase separation Methods 0.000 abstract description 3
- 230000005415 magnetization Effects 0.000 description 18
- 230000008021 deposition Effects 0.000 description 11
- 238000010586 diagram Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000004544 sputter deposition Methods 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000004813 Moessbauer spectroscopy Methods 0.000 description 1
- 238000001669 Mossbauer spectrum Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000001941 electron spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Magnetic Record Carriers (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Thin Magnetic Films (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
（イ）産業上の利用分野
本発明は窒化鉄または窒化鉄系合金からなる強磁性金属
薄膜を磁性層とする垂直磁気記録媒体及びその製造方法
に関する。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application The present invention relates to a perpendicular magnetic recording medium whose magnetic layer is a ferromagnetic metal thin film made of iron nitride or an iron nitride alloy, and a method for manufacturing the same.
（ロ）従来の技術
東北大の岩崎らにより発表された垂直磁気記録は、記録
密度が高くなるほど自己減磁作用が抑制されるため本質
的に高密度記録に適した記録方式である。垂直磁気記録
用の媒体としては、スパッタ法もしくは真空蒸着法で作
製したＣｏ−Ｃｒ膜が発表されている。(b) Conventional technology The perpendicular magnetic recording announced by Iwasaki et al. of Tohoku University is essentially a recording method suitable for high-density recording because self-demagnetization is suppressed as the recording density increases. As a medium for perpendicular magnetic recording, a Co--Cr film produced by a sputtering method or a vacuum evaporation method has been announced.
Ｃｏ−Ｃｒ膜は磁気異方性、飽和磁化ともに大きく垂直
記録媒体として優れているが、Ｃｏはコスト的に高価な
ため問題がある。上述の欠点を解消したものとして、例
えば特開昭５９−２２８７０５号（１（ＯＩＦＩＯ／１
８）に開示されているように、安価なＦｅをベースにし
たＦｅＮ系垂直磁気記録媒体が提案されている。これは
大方晶系窒化鉄（ε−Ｆｅｅｍ。Although a Co--Cr film has large magnetic anisotropy and saturation magnetization and is excellent as a perpendicular recording medium, Co has a problem because it is expensive. For example, Japanese Patent Application Laid-Open No. 59-228705 (1 (OIFIO/1)
8), an inexpensive FeN-based perpendicular magnetic recording medium based on Fe has been proposed. This is orthogonal iron nitride (ε-Feem).
Ｎ）を主体とする媒体であり、鉄、７’−Ｆｅ４Ｎ、ｔ
−Ｆ、ｅｍ−２Ｎ、ζ−Ｆｅ２ＮのようなＦｅまたはそ
の窒化物の中から選ばれた少なくとも１つの粉末、粉末
焼結体、バルクを原料として、Ａｒ気流中、Ａｒと窒素
の混合気流中、もしくはＡｒ、窒素、水素の混合気流中
で物理蒸着（スパッタ法、真空蒸着法）を行うことによ
り形成される。N), iron, 7'-Fe4N, t
- At least one powder, powder sintered body, or bulk selected from Fe or its nitrides such as -F, em-2N, and ζ-Fe2N is used as a raw material in an Ar gas flow or a mixed gas flow of Ar and nitrogen. Alternatively, it is formed by physical vapor deposition (sputtering method, vacuum evaporation method) in a mixed gas flow of Ar, nitrogen, and hydrogen.
しかし乍ら、上述のような六方晶系窒化鉄を主体とする
薄膜磁性体では、磁性層を高速で形成することが出来ず
、量産性に適した磁気記録媒体ではなかった。However, with the thin film magnetic material mainly composed of hexagonal iron nitride as described above, the magnetic layer cannot be formed at high speed, and the magnetic recording medium is not suitable for mass production.
（ハ）発明が解決しようとする課題
本発明は上記従来例の欠点に鑑み為されたものであり、
高速で形成可能な垂直磁気異方性を有する窒化鉄系の磁
性層を有する垂直磁気記録媒体及びその製造方法を提供
することを目的とするものである。(c) Problems to be Solved by the Invention The present invention has been made in view of the drawbacks of the above-mentioned conventional examples.
It is an object of the present invention to provide a perpendicular magnetic recording medium having an iron nitride-based magnetic layer having perpendicular magnetic anisotropy that can be formed at high speed, and a method for manufacturing the same.
（ニ）課題を解決するための手段
本発明の垂直磁気記録媒体は、非磁性の基板上に常磁性
窒化鉄ζ−ＦｅｔＮを主体とし、結晶構造が前記基板上
面に対して垂直方向に延びる柱状構造である垂直磁気異
方性を有するＦｅＮ系磁性薄膜を被着形成したことを特
徴とする。(d) Means for Solving the Problems The perpendicular magnetic recording medium of the present invention is mainly composed of paramagnetic iron nitride ζ-FetN on a non-magnetic substrate, and has a columnar crystal structure extending perpendicularly to the upper surface of the substrate. It is characterized in that a FeN-based magnetic thin film having perpendicular magnetic anisotropy is deposited thereon.
また、本発明の垂直磁気記録媒体の製造方法は、加熱さ
れた非磁性の基板上に該基板上面と直交する方向から鉄
の蒸気を蒸着すると同時に、該蒸着部に窒素イオン及び
電子を含有する窒素プラズマを照射することにより前記
基板上に常磁性窒化鉄ζ−Ｆｅ＊Ｎを主体とする垂直磁
気異方性を有するＦｅＮ系磁性薄膜を被着形成すること
を特徴とする。Further, in the method for manufacturing a perpendicular magnetic recording medium of the present invention, iron vapor is deposited onto a heated non-magnetic substrate from a direction perpendicular to the upper surface of the substrate, and at the same time, nitrogen ions and electrons are contained in the deposited portion. The present invention is characterized in that an FeN-based magnetic thin film having perpendicular magnetic anisotropy and mainly composed of paramagnetic iron nitride ζ-Fe*N is deposited on the substrate by irradiating nitrogen plasma.
（ホ）作 用
上記構造の垂直磁気記録媒体では、常磁性窒化鉄ζ−Ｆ
ｅ２Ｎの結晶化に伴いフェロ磁性のα−Ｆｅ相及びγ’
−Ｆｅ２Ｎ相との相分離に磁気的分離効果が起こり、こ
れが基板上面に対して垂直方向に延びた微細柱状構造に
よる形状異方性と相乗することにより垂直磁気異方性の
優れたＦｅＮ系磁性薄膜が形成される。(e) Effect In the perpendicular magnetic recording medium with the above structure, paramagnetic iron nitride ζ-F
As e2N crystallizes, ferromagnetic α-Fe phase and γ'
-A magnetic separation effect occurs during phase separation with the Fe2N phase, and this synergy with the shape anisotropy due to the fine columnar structure extending perpendicularly to the top surface of the substrate results in FeN-based magnetism with excellent perpendicular magnetic anisotropy. A thin film is formed.
また、上述の製造方法では、プラズマ生成室からの低い
運動ヱネルギー領域でのイオン照射と適当な基板温度と
の相互作用により常磁性窒化鉄ζ−Ｆ ｅ ＊Ｎの結晶
化が進む。Furthermore, in the above-described manufacturing method, crystallization of paramagnetic iron nitride ζ-Fe*N progresses due to interaction between ion irradiation from the plasma generation chamber in a low kinetic energy region and an appropriate substrate temperature.
（へ）実施例
第１図は本実施例で用いられるイオンアシスト蒸着法に
よる垂直磁気記録媒体の製造装置の概略断面図である。(F) Embodiment FIG. 1 is a schematic cross-sectional view of an apparatus for manufacturing a perpendicular magnetic recording medium by the ion-assisted vapor deposition method used in this embodiment.
図中、（１）は排気系（２）により内部がｌＸｌ０−’
Ｔ ｏ ｒ ｒ以下の高真空に保たれた真空槽であり、
該真空槽（１）の内部にはるつぼ（３）、基板ホルダー
（４）及びプラズマ生成室（且）が配設されている。前
記るつぼ（３）内には蒸発源である鉄（６）が収納され
ている。前記基板ホルダー（４）の下面には非磁性の基
板（７）が装着されており、該基板（７）の真下に前記
るつぼ（３）が配置されている。In the figure, (1) is internally lXl0-' due to the exhaust system (2).
It is a vacuum chamber maintained at a high vacuum below T o r r,
A crucible (3), a substrate holder (4), and a plasma generation chamber (and) are arranged inside the vacuum chamber (1). Iron (6), which is an evaporation source, is housed in the crucible (3). A non-magnetic substrate (7) is mounted on the lower surface of the substrate holder (4), and the crucible (3) is placed directly below the substrate (7).
また、前記基板ホルダー（４）の角部にはヒータ（図示
せず）が装着されており、該ヒータにより前記基板（７
）の温度が制御される。前記プラズマ生成室（５）は内
部にフィラメント（８）及びアノード（９）が装着され
ており、周面にはソレノイドコ・イル（１０）が巻回さ
れている。前記フィラメント（８）には直流電源（ｌｌ
ａ）により２０〜３０Ａの電流が流れており、前記アノ
ード（９）には直流電源（１１ｂ）により１００ｖの正
の電圧が印加されている。Further, a heater (not shown) is attached to a corner of the substrate holder (4), and the heater causes the substrate (7) to
) temperature is controlled. A filament (8) and an anode (9) are installed inside the plasma generation chamber (5), and a solenoid coil (10) is wound around the circumferential surface. The filament (8) is connected to a DC power source (ll
A current of 20 to 30 A is flowing through a), and a positive voltage of 100 V is applied to the anode (9) by a DC power source (11b).
また、前記プラズマ生成室（互）のプラズマ（１２）放
出側の開口部には電気的に接地された多孔形状のグリッ
ド（１３）が装着されており、該グリッド（１３）によ
りプラズマ生成室（５）の内外には気圧差が生じる。（
１４）は前記プラズマ生成室（互）の内部に窒素ガスを
導入するためのガス導入管である。Further, an electrically grounded porous grid (13) is attached to the opening on the plasma (12) emission side of the plasma generation chamber (12), and the grid (13) allows the plasma generation chamber (12) to 5) There is a difference in air pressure between the inside and the outside. (
14) is a gas introduction pipe for introducing nitrogen gas into the plasma generation chamber.
上述の本実施例の製造装置では、ガス導入管（１４）を
通ってプラズマ生成室（互）内に導入された中性の窒素
分子は、フィラメント（８〉から放出されアノード（９
）によって加速された熱電子と衝突することによりイオ
ン化される。このイオン化により発生した低エネルギー
の窒素イオンと電子とは、窒素プラズマ（１２）となり
、ソレノイドコイル（１０）により形成された磁場匂配
とグリッド（１３）による気圧差とによってプラズマ生
成室（５）の開口部から外部に放射状に放出される。こ
の放出された窒素プラズマ（１２）はるつぼ（３）から
の鉄の蒸気（１４）と同時に基板（７）に照射される。In the manufacturing apparatus of this embodiment described above, the neutral nitrogen molecules introduced into the plasma generation chamber through the gas introduction pipe (14) are emitted from the filament (8>) and are passed through the anode (9).
) is ionized by collision with thermal electrons accelerated by The low-energy nitrogen ions and electrons generated by this ionization become nitrogen plasma (12), which is generated in a plasma generation chamber (5) by the magnetic field generated by the solenoid coil (10) and the pressure difference caused by the grid (13). is emitted radially to the outside from the opening. This emitted nitrogen plasma (12) is irradiated onto the substrate (7) at the same time as the iron vapor (14) from the crucible (3).
このため、前記基板（７）に到達した窒素イオンの正の
電荷は電子によって中和され、前記基板（７）はチャー
ジアップしない。また、前記窒素イオン及び電子の運動
エネルギーは１００ｅＶ以下と小さいので基板（７）上
に形成された窒化鉄（ＦｅＮ）磁性薄膜は熱解離を生じ
ない。Therefore, the positive charge of the nitrogen ions reaching the substrate (7) is neutralized by electrons, and the substrate (7) is not charged up. Furthermore, since the kinetic energy of the nitrogen ions and electrons is as small as 100 eV or less, the iron nitride (FeN) magnetic thin film formed on the substrate (7) does not undergo thermal dissociation.
上述の製造装置を使用して下記の条件でフィルム基板上
にＦｅＮ磁性薄膜を形成した。An FeN magnetic thin film was formed on a film substrate using the above manufacturing apparatus under the following conditions.
−成膜条件−
背圧 ｌＸｌ０−＠ｔｏｒｒ以下窒素ガ
ス圧力 ２Ｘ１０−’ｔｏｒｒ戊膜速度成膜
７５０〜１７５０Ａ／ ｍ ｉ ｎ窒素イオン電流
密度 ２ 、０ ｍ Ａ ／ ｃ ｍ ’鉄蒸気
の入射角 ９０”フィルム基板温
度 ｉｏｏ℃窒素イオンの運動エネル
ギー １００ｅＶ以下上述の成膜条件で形成されたＦｅ
Ｎ磁性薄膜の磁気特性の成膜速度依存性を第２図、第３
図及び第４図に示す。第２図は飽和磁化Ｍｓの成膜速度
依存性と、垂直方向ヒ面内方向この残留磁化比Ｂｒ土／
Ｂ ｒ 、の成膜速度依存性とを示す図、第３図は垂
直磁気異方性磁界Ｈｋの成膜速度依存性を示す図、第４
図は垂直保磁力Ｈｃ 、Ｌの成膜速度依存性を示す図で
ある。-Film forming conditions- Back pressure 1Xl0-@torr or less Nitrogen gas pressure 2X10-'torr Film-forming rate 750-1750A/min Nitrogen ion current density 2, 0 mA/cm' Incident angle of iron vapor 90 "Film substrate temperature: ioo℃Nitrogen ion kinetic energy: 100eV or less Fe formed under the above film formation conditions
Figures 2 and 3 show the dependence of the magnetic properties of the N magnetic thin film on the deposition rate.
It is shown in FIG. Figure 2 shows the dependence of the saturation magnetization Ms on the deposition rate and the residual magnetization ratio Br soil/in the perpendicular direction and the in-plane direction.
FIG. 3 is a diagram showing the dependence of the perpendicular magnetic anisotropy field Hk on the deposition rate; FIG.
The figure shows the dependence of the perpendicular coercive force Hc, L on the film formation rate.
第２図、第３図及び第４図から判るように成膜速度を１
７５ ＯＡ／ｍ ｉ ｎから減少させていくに従い、垂
直方向と面内方向との残留磁化比Ｂｒ上／ Ｂ ｒ 、
、垂直磁気異方性磁界Ｈｋ、垂直保持力Ｈｅ上等の垂直
磁化特性が向上し、成膜速度が１０００Ａ／ｍｉｎでは
、飽和磁化Ｍｓが２９０ｅ ｍ ｕ ／ ｅ ｃ、垂直
方向と面内方向との残留磁化比Ｂｒ上／ Ｂ ｒ 、が
１．２、垂直磁気異方性磁界Ｈｋが２８０００ｅ、垂直
保磁力Ｈｅ土が４５００ｅという良好な垂直磁化特性が
得られた。As can be seen from Figures 2, 3, and 4, the deposition rate was increased to 1.
As it decreases from 75 OA/min, the residual magnetization ratio Br in the vertical direction and in the in-plane direction increases / Br,
, perpendicular magnetic anisotropy magnetic field Hk, perpendicular coercive force He, and other perpendicular magnetization characteristics are improved, and at a deposition rate of 1000 A/min, the saturation magnetization Ms is 290 e m u / e c, both in the perpendicular direction and in-plane direction. Good perpendicular magnetization characteristics were obtained, with a remanent magnetization ratio Br/Br of 1.2, a perpendicular magnetic anisotropy field Hk of 28000e, and a perpendicular coercivity He soil of 4500e.
第５図は上述の成膜条件の成膜速度１７５０Ａ／ ｍ
ｉ ｎで形成されたＦｅＮ磁性薄膜の結晶構造を示す走
査型電子顕微鏡写真、第６図は上述の成膜条件の成膜速
度１０００Ａ／ｍｉｎで形成されたＦｅＮ磁性薄膜の結
晶構造を示す走査型電子顕微鏡写真である。Figure 5 shows a film forming rate of 1750 A/m under the above film forming conditions.
Figure 6 is a scanning electron micrograph showing the crystal structure of the FeN magnetic thin film formed under the above-mentioned film forming conditions at a deposition rate of 1000 A/min. This is an electron micrograph.
第５図及び第６図から判るように成膜速度１７５０人／
ｍ ｉ ｎで形成されたＦｅＮ磁性薄膜には柱状構造
の結晶構造が見られなかったのに対し、良好な垂直磁化
特性が得られた成膜速度１０００入で形成されたＦｅＮ
磁性薄膜では、垂直方向に延びる柱状構造の結晶構造が
形成される。As can be seen from Figures 5 and 6, the deposition rate was 1750 people/
No columnar crystal structure was observed in the FeN magnetic thin film formed at min, whereas the FeN magnetic thin film formed at a deposition rate of 1000 mm, which yielded good perpendicular magnetization characteristics,
In the magnetic thin film, a columnar crystal structure extending in the vertical direction is formed.
第７図は上述の成膜条件の成膜速度１７５０Ａ／ ｍ
ｉ ｎで形成されたＦｅＮ磁性薄膜のＸ線回折による組
成分析の結果を示す図、第８図は上述の成膜条件の成膜
速度１ｏｏｏ人／ ｍ ｉ ｎで形成されたＦｅＮ磁性
薄膜のＸ線回折による組成分析の結果を示す図である。Figure 7 shows a film forming rate of 1750 A/m under the above film forming conditions.
Figure 8 shows the results of compositional analysis by X-ray diffraction of the FeN magnetic thin film formed under the above-mentioned film formation conditions. FIG. 3 is a diagram showing the results of compositional analysis by line diffraction.
第７図及び第８図から判るように成膜速度１７５０人／
ｍ ｉ ｎで形成されたＦｅＮ磁性薄膜の回折パター
ンが７−’−Ｆｅ４Ｎとε−Ｆ ｅ ｔ〜２Ｎというフ
ェロ磁性相の混合パターンであるのに対し、良好な垂直
磁化特性が得られた成膜速度１０００Ａ ／ ｍ ｉ
ｎで形成されたＦｅＮ磁性薄膜ではζ−Ｆｅ＊Ｎのみの
回折パターンを示した。As can be seen from Figures 7 and 8, the deposition rate was 1750 people/
The diffraction pattern of the FeN magnetic thin film formed by min is a mixed pattern of ferromagnetic phases of 7-'-Fe4N and ε-Fet~2N, whereas the Film speed 1000A/mi
The FeN magnetic thin film formed with n showed a diffraction pattern of only ζ-Fe*N.
第９図は良好な垂直磁化特性か得られた成膜速度１００
０Ａ／ ｍ ｉ ｎで形成されたＦｅＮ磁性薄膜のメス
バウア分光による組成分析の結果を示す図であり、この
図から上記ＦｅＮ磁性薄膜の組成が下記の通り判明した
。Figure 9 shows the film formation rate of 100 that resulted in good perpendicular magnetization characteristics.
FIG. 2 is a diagram showing the results of composition analysis by Mössbauer spectroscopy of a FeN magnetic thin film formed at 0 A/min, and from this diagram, the composition of the FeN magnetic thin film was found as follows.
−ＦｅＮ磁性薄膜の組成−
常磁性（室温） ζ−Ｆｅ２Ｎ ６２％常磁性
（室温） ｔ−Ｆｅ、−２Ｎ ２２％強磁性（
室温） α−Ｆｅ ８％強磁性（室温）
γ’ ＦｅｔＮ ８％また、このＦｅＮ磁
性薄膜の磁化が強磁性のα−Ｆｅとγ’−Ｆｅ２Ｎに帰
属していることが判る。-Composition of FeN magnetic thin film- Paramagnetic (room temperature) ζ-Fe2N 62% paramagnetic (room temperature) t-Fe, -2N 22% ferromagnetic (
(room temperature) α-Fe 8% ferromagnetic (room temperature)
γ' FetN 8% It can also be seen that the magnetization of this FeN magnetic thin film belongs to ferromagnetic α-Fe and γ'-Fe2N.
また、上述の成膜条件で形成されたＦｅＮ磁性薄膜の窒
素含有量を電子分光法により調べると、成膜速度を減少
させていくに従い窒素含有量は増加し、良好な垂直磁化
特性が得られた成膜速度１０００Ａ／ｍ ｉ ｎでの窒
素含有量が２３ａｔｍ％であることが判った。Furthermore, when the nitrogen content of the FeN magnetic thin film formed under the above-mentioned film-forming conditions was investigated by electron spectroscopy, the nitrogen content increased as the film-forming rate decreased, and good perpendicular magnetization characteristics were obtained. It was found that the nitrogen content was 23 atm % at a film formation rate of 1000 A/min.
次に、上述の成膜条件において、成膜速度を１０００Ａ
／ ｍ ｉ ｎに固定し基板温度を４０℃〜２４０℃ま
で変化させて形成されたＦｅＮ磁性薄膜の磁気特性の基
板温度依存性を第１０図及び第１１図に示す。第１０図
は飽和磁化Ｍｓの基板温度依存性と垂直方向と面内方向
との残留磁化比Ｂｒ上／ Ｂ ｒ 、の基板温度依存性
とを示す図、第１１図は垂直磁気異方性磁界Ｈｋの基板
温度依存性を示す図である。Next, under the above film forming conditions, the film forming rate was set to 1000 A.
FIGS. 10 and 11 show the dependence of the magnetic properties on the substrate temperature of FeN magnetic thin films formed by fixing the temperature at / min and varying the substrate temperature from 40° C. to 240° C. Fig. 10 is a diagram showing the substrate temperature dependence of the saturation magnetization Ms and the substrate temperature dependence of the remanent magnetization ratio Br/Br in the perpendicular direction and in-plane direction, and Fig. 11 is a diagram showing the dependence of the saturation magnetization Ms on the substrate temperature. FIG. 3 is a diagram showing the substrate temperature dependence of Hk.
第１０図及び第１１図から判るように、垂直方向と面内
方向との残留磁化比Ｂｒ上／ Ｂ ｒ 、、垂直磁気異
方性磁界Ｈｋ等の垂直磁化特性は基板温度１００℃近傍
で形成されたＦｅＮ磁性薄膜が最も良好な値を示してい
る。As can be seen from Figures 10 and 11, perpendicular magnetization characteristics such as the remanent magnetization ratio Br in the vertical direction and the in-plane direction Br/Br, and the perpendicular magnetic anisotropy field Hk are formed at a substrate temperature of around 100°C. The FeN magnetic thin film shown in Fig. 1 shows the best value.
上述の基板温度１００℃、成膜速度１０００Ａ／ ｍ
ｉ ｎの条件で形成した実施例のＦｅＮ磁性薄膜は、基
板（７）上面に対して垂直方向に成長した微細柱状構造
のフェロ磁性のα−Ｆｅ相及びγ′−Ｆ ｅ ４Ｎ相の
結晶の周りで、プラズマ生成室（５）からの１００ｅＶ
以下の低い運動エネルギー領域でのイオン照射と１００
℃の基板温度との相互作用により常磁性のζ−Ｆｅ＊Ｎ
が結晶化することにより前記α−Ｆｅ相とγ’−Ｆｅ４
Ｎ相との相分離に磁気的分離効果が起こり、これが前記
微細柱状構造による形状異方性と相乗することにより優
れた垂直磁気異方性を示す。Above substrate temperature 100°C, film formation rate 1000A/m
The FeN magnetic thin film of the example formed under the conditions of i. around 100 eV from the plasma generation chamber (5)
Ion irradiation in the low kinetic energy region below and 100
Paramagnetic ζ-Fe*N due to interaction with substrate temperature of °C
is crystallized to form the α-Fe phase and γ'-Fe4
A magnetic separation effect occurs during phase separation with the N phase, and this synergy with the shape anisotropy due to the fine columnar structure provides excellent perpendicular magnetic anisotropy.
また、比較例として、第１２図に示す通常の真空蒸着装
置を用いて下記の条件で、基板（７）上にＦｅＮ磁性薄
膜を形成した。Further, as a comparative example, a FeN magnetic thin film was formed on the substrate (7) using a normal vacuum evaporation apparatus shown in FIG. 12 under the following conditions.
一成膜条件一
背Ｅ ｌＸｌ０−”ｔｏｒｒ以下窒素
ガス圧力 ２×１０引ｔｏｒｒ戊膜速度
１０００Ａ／ｍｉｎ窒素イオン電流密度
Ｏｍ Ａ ／ ｃ ｍ ”鉄蒸気の入射角
９０”フィルム基板温度
ｉｏｏ℃窒素イオンの運動エネルギー Ｏ
ｅＶ下表に上述の実施例（成膜速度１０００Å／ｍｉｎ
、基板温度１００℃）で形成したＦｅＮ磁性薄膜と上述
の比較例で形成したＦｅＮ磁性薄膜の磁気特性を示す。Film forming conditions: E lXl0-” torr or less Nitrogen gas pressure 2×10 torr Filming speed
1000A/min nitrogen ion current density
Om A/cm ”Angle of incidence of iron vapor
90” film substrate temperature
ioo°C Kinetic energy of nitrogen ions O
eV The table below shows the above examples (deposition rate 1000 Å/min
The magnetic properties of the FeN magnetic thin film formed at a substrate temperature of 100° C. and the FeN magnetic thin film formed in the above-mentioned comparative example are shown.
以下余白
また、上述の比較例で形成されたＦｅＮ磁性薄膜の走査
型電子顕微鏡での観察では柱状構造の結晶構造は見られ
ず、またＸ線回折による組成分析ではα−Ｆｅの回折パ
ターンのみが見られた。Margin below In addition, when the FeN magnetic thin film formed in the above-mentioned comparative example was observed with a scanning electron microscope, no columnar crystal structure was observed, and when the composition was analyzed by X-ray diffraction, only the α-Fe diffraction pattern was observed. It was seen.
また、他の比較例として第１図の製造装置において基板
ホルダー（４）を所定角度傾けて鉄を斜め蒸着して基板
（７）上にＦｅＮ磁性薄膜を形成した。このＦｅＮ系磁
性薄膜は第１３図に示すように基板上面に対して斜め上
方に成長じた柱状構造の結晶構造を有しており、窒素含
有量は１６ａｔｍ％である。しかし乍ら、この比較例の
ＦｅＮ磁性薄膜は垂直方向と面内方向の残留磁化比Ｂｒ
上／ Ｂ ｒ 、は０．３０程度であり、はとんど垂直
磁気異方性を有していない。尚、上述の第５図、第６図
及び第１３図の走査型電子顕微鏡写真では１ｃｒｎ＝１
６６０人の倍率である。As another comparative example, a FeN magnetic thin film was formed on the substrate (7) by tilting the substrate holder (4) at a predetermined angle and depositing iron obliquely in the manufacturing apparatus shown in FIG. As shown in FIG. 13, this FeN-based magnetic thin film has a columnar crystal structure grown obliquely upward from the upper surface of the substrate, and has a nitrogen content of 16 atm %. However, the FeN magnetic thin film of this comparative example has a residual magnetization ratio Br in the vertical direction and in the in-plane direction.
The upper /B r is about 0.30, and has almost no perpendicular magnetic anisotropy. In addition, in the above-mentioned scanning electron micrographs of FIGS. 5, 6, and 13, 1crn=1
This is a multiple of 660 people.
（ト）発明の効果
本発明に依れば、量産性に適した垂直磁気記録媒体及び
その製造方法を提供し得る。(G) Effects of the Invention According to the present invention, it is possible to provide a perpendicular magnetic recording medium suitable for mass production and a method for manufacturing the same.
第１図乃至第１１図は本発明に係り、第１図は製造装置
の概略断面図、第２図、第３図及び第４図は夫々ＦｅＮ
磁性薄膜の磁気特性の成膜速度依存性を示す図、第５図
及び第６図は夫々ＦｅＮ磁性薄膜の結晶構造を示す走査
型電子顕微鏡写真、第７図及び第８図は夫々ＦｅＮ磁性
薄膜のＸ線回折パターンを示す図、第９図はＦｅＮ磁性
薄膜のメスバウアスペクトルを示す図、第１０図及び第
１１図は夫々ＦｅＮ磁性薄膜の磁気特性の基板温度依存
性を示す図である。第１２図は製造装置の概略断面図、
第１３図はＦｅＮ磁性薄膜の結晶構造を示す走査型電子
顕微鏡写真である。
（５）・・・プラズマ生成基、（７）・・・基板、（１
２）・・・窒素プラズマ、（１４）・・・鉄の蒸気。1 to 11 relate to the present invention, FIG. 1 is a schematic cross-sectional view of a manufacturing apparatus, and FIGS. 2, 3, and 4 are FeN
Figures 5 and 6 are scanning electron micrographs showing the crystal structure of FeN magnetic thin films. Figures 7 and 8 are scanning electron micrographs showing the deposition rate dependence of magnetic properties of magnetic thin films. FIG. 9 is a diagram showing the Mössbauer spectrum of the FeN magnetic thin film, and FIGS. 10 and 11 are diagrams showing the substrate temperature dependence of the magnetic properties of the FeN magnetic thin film. FIG. 12 is a schematic cross-sectional view of the manufacturing equipment;
FIG. 13 is a scanning electron micrograph showing the crystal structure of the FeN magnetic thin film. (5)...Plasma generation group, (7)...Substrate, (1
2)...Nitrogen plasma, (14)...Iron vapor.
Claims (2)
主体とし、結晶構造が前記基板上面に対して垂直方向に
延びる柱状構造である垂直磁気異方性を有するＦｅＮ系
磁性薄膜を被着形成したことを特徴とする垂直磁気記録
媒体。(1) A FeN-based magnetic thin film mainly composed of paramagnetic iron nitride ζ-Fe_2N and having perpendicular magnetic anisotropy, whose crystal structure is a columnar structure extending perpendicularly to the upper surface of the substrate, is coated on a nonmagnetic substrate. 1. A perpendicular magnetic recording medium characterized in that it has an adhesive layer.
る方向から鉄の蒸気を蒸着すると同時に、該蒸着部に窒
素イオン及び電子を含有する窒素プラズマを照射するこ
とにより前記基板上に常磁性窒化鉄ζ−Ｆｅ＿２Ｎを主
体とする垂直磁気異方性を有するＦｅＮ系磁性薄膜を被
着形成することを特徴とする垂直磁気記録媒体の製造方
法。(2) Depositing iron vapor onto a heated non-magnetic substrate from a direction perpendicular to the upper surface of the substrate, and at the same time irradiating the vapor deposition area with nitrogen plasma containing nitrogen ions and electrons. 1. A method for manufacturing a perpendicular magnetic recording medium, which comprises depositing a FeN-based magnetic thin film having perpendicular magnetic anisotropy mainly composed of paramagnetic iron nitride ζ-Fe_2N.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1208130A JP2752179B2 (en) | 1989-08-10 | 1989-08-10 | Perpendicular magnetic recording medium and method of manufacturing the same |
| US07/564,256 US5173370A (en) | 1989-08-10 | 1990-08-08 | Magnetic recording medium having a magnetic thin film with both paramagnetic phase and ferromagnetic phase iron nitride with paramagnetic phase zeta Fe2 N as its largest component |
| EP90115388A EP0415155B1 (en) | 1989-08-10 | 1990-08-10 | A perpendicular magnetic recording medium and method of forming the same |
| DE69023835T DE69023835T2 (en) | 1989-08-10 | 1990-08-10 | Vertical magnetic recording medium and method for the production thereof. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1208130A JP2752179B2 (en) | 1989-08-10 | 1989-08-10 | Perpendicular magnetic recording medium and method of manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0371420A true JPH0371420A (en) | 1991-03-27 |
| JP2752179B2 JP2752179B2 (en) | 1998-05-18 |
Family
ID=16551134
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1208130A Expired - Fee Related JP2752179B2 (en) | 1989-08-10 | 1989-08-10 | Perpendicular magnetic recording medium and method of manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2752179B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7336293B2 (en) | 2000-10-30 | 2008-02-26 | Yamaha Corporation | Scanning optical media during label printing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57130405A (en) * | 1981-02-05 | 1982-08-12 | Semiconductor Energy Lab Co Ltd | Magnetic recording medium |
| JPS6025204A (en) * | 1983-07-20 | 1985-02-08 | Konishiroku Photo Ind Co Ltd | Megnetic recording medium |
| JPH01105331A (en) * | 1987-04-15 | 1989-04-21 | Sanyo Electric Co Ltd | Production of magnetic recording medium |
-
1989
- 1989-08-10 JP JP1208130A patent/JP2752179B2/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57130405A (en) * | 1981-02-05 | 1982-08-12 | Semiconductor Energy Lab Co Ltd | Magnetic recording medium |
| JPS6025204A (en) * | 1983-07-20 | 1985-02-08 | Konishiroku Photo Ind Co Ltd | Megnetic recording medium |
| JPH01105331A (en) * | 1987-04-15 | 1989-04-21 | Sanyo Electric Co Ltd | Production of magnetic recording medium |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7336293B2 (en) | 2000-10-30 | 2008-02-26 | Yamaha Corporation | Scanning optical media during label printing |
| US7336292B2 (en) | 2000-10-30 | 2008-02-26 | Yamaha Corporation | Optical media label printing using different power levels |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2752179B2 (en) | 1998-05-18 |
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