JPS63255813A - Perpendicular magnetic recording medium - Google Patents
Perpendicular magnetic recording mediumInfo
- Publication number
- JPS63255813A JPS63255813A JP9055987A JP9055987A JPS63255813A JP S63255813 A JPS63255813 A JP S63255813A JP 9055987 A JP9055987 A JP 9055987A JP 9055987 A JP9055987 A JP 9055987A JP S63255813 A JPS63255813 A JP S63255813A
- Authority
- JP
- Japan
- Prior art keywords
- film
- segregation
- magnetic film
- sputtering
- average
- 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
- 238000005204 segregation Methods 0.000 claims abstract description 37
- 238000004544 sputter deposition Methods 0.000 abstract description 24
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 230000005415 magnetization Effects 0.000 abstract description 9
- 238000007740 vapor deposition Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 42
- 239000000758 substrate Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910000599 Cr alloy Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006866 deterioration Effects 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
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- -1 that is Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、膜面に対し垂直方向の磁化によって情報記録
がなされる垂直磁気記録媒体、特にＣｏ −Ｃｒ系磁性
膜による例えばオーディオ用、ビデオ用、コンピュータ
用の垂直磁気記録媒体に関わる。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to perpendicular magnetic recording media in which information is recorded by magnetization in a direction perpendicular to the film surface, particularly for use in audio, video, etc., using a Co-Cr magnetic film. Related to perpendicular magnetic recording media for computers.
本発明は、膜面に沿う方向に関してのＣｒの偏析領域の
配置状態が、その平均配置周期が３０Å〜３００人をも
って形成されたＧｏ−Ｃｒ系磁性膜を有して成り、垂直
方向の磁気特性、特に保磁力ＨＩＪの向上をはかる。The present invention has a Go-Cr-based magnetic film in which the arrangement state of Cr segregation regions in the direction along the film surface has an average arrangement period of 30 Å to 300, and has magnetic properties in the perpendicular direction. In particular, the coercive force HIJ is improved.
Ｇｏ−Ｃｒ系磁性膜による磁気記録媒体は、蒸着もしく
はスパッタリングによって６万晶形の柱状結晶粒が膜面
に対し垂直方向に配向して形成することができることか
ら垂直磁気特性にすぐれており、垂直磁気記録媒体とし
て脚光を浴びるに至ってし）る。A magnetic recording medium using a Go-Cr magnetic film has excellent perpendicular magnetic properties because it can be formed by vapor deposition or sputtering with 60,000 crystal columnar crystal grains oriented perpendicularly to the film surface. It has come into the spotlight as a recording medium).
そして、このＣｏ−Ｃｒ系垂直磁気記録媒体において、
より高い磁気特性、例えばより高し）垂直方向保磁力）
１ｃＡを得るための研究開発がなお進められているとこ
ろである。しかしながら、このＣｏ−Ｃｒ系磁性膜にお
ける磁気特性が、何に起因して変化するものであるかは
、未だ充分解明されていないところであり、一般には、
ｈ、ｃ、ｐ、相のＣ軸配向、或いは柱状構造に関係する
と考えられてはいるものの、これだけでは充分に特性の
説明をなし得ない。In this Co-Cr-based perpendicular magnetic recording medium,
Higher magnetic properties, e.g. higher vertical coercivity)
Research and development to obtain 1cA is still underway. However, it is still not fully understood what causes the magnetic properties of this Co-Cr magnetic film to change, and in general,
Although it is believed that this is related to the C-axis orientation of the h, c, p, phase, or the columnar structure, this alone cannot fully explain the characteristics.
近年、Ｃｒの偏析が垂直保磁力ＨＣＩや、実効的垂直磁
気異方性定数Ｈｋｅｆｆを向上させるための重要な要因
であるとして注目されて来てはいるものの、このＣｒの
偏析は、通常Ｃｏ−Ｃｒ柱状結晶の表面、すなわち結晶
磁界での偏析である０例えば特公昭６１−５３７７０号
公報に開示された垂直磁気記録媒体においても結晶粒表
面にＣｒを偏析させるものであって、この場合耐蝕性の
向上をはかっているものである。In recent years, Cr segregation has attracted attention as an important factor for improving the perpendicular coercive force HCI and the effective perpendicular magnetic anisotropy constant Hkeff, but this Cr segregation is usually For example, in the perpendicular magnetic recording medium disclosed in Japanese Patent Publication No. 61-53770, Cr is segregated on the surface of the crystal grains, and in this case, corrosion resistance is The aim is to improve the
しかしながら、このように結晶粒の表面、すなわち結晶
粒界にＣｒの偏析を行わせる場合、垂直磁気特性の向上
がはかられるとはいうものの、未だ実際に望まれる程度
に高い磁気特性は得られていない。However, although the perpendicular magnetic properties are improved when Cr is segregated on the surface of the crystal grains, that is, on the grain boundaries, it is still not possible to obtain magnetic properties as high as actually desired. Not yet.
一方、例えば特開昭５９−１２９９３４号公報には、Ｃ
。On the other hand, for example, in Japanese Patent Application Laid-open No. 59-129934, C.
.
−Ｃｒ系垂直磁化膜にカーボンを０．５％以上含有させ
てＣ軸配向を高めることの開示がある。There is a disclosure that the C-axis orientation is enhanced by containing 0.5% or more of carbon in a -Cr-based perpendicularly magnetized film.
また、特開昭６０−２４６０１６号公開公報には、Ｃｏ
−Ｃｒ系磁性膜の耐久性を向上する目的をもってカー
ボンＣを０．０１〜１．０重量％（０，０５〜４原子％
）添加したＣｏ −Ｃｒ系合金薄膜によって垂直磁気記
録膜を形成することの開示がある。しかしながら、この
場合、飽和磁化が減少するという現象が生じている。Also, in Japanese Patent Application Laid-open No. 60-246016, Co
- Carbon C is added in an amount of 0.01 to 1.0% by weight (0.05 to 4 atomic%) for the purpose of improving the durability of the Cr-based magnetic film.
) There is a disclosure of forming a perpendicular magnetic recording film using a Co--Cr based alloy thin film added. However, in this case, a phenomenon occurs in which the saturation magnetization decreases.
本発明は、Ｃｏ−Ｃｒ系磁性膜を有する垂直磁気記録媒
体において、垂直磁気特性、特に垂直保磁力ＵＣ工の問
題、飽和磁化Ｍｓの問題の解決をはかる。The present invention aims to solve the perpendicular magnetic properties, particularly the problems of perpendicular coercive force UC and saturation magnetization Ms, in a perpendicular magnetic recording medium having a Co--Cr magnetic film.
本発明は、結晶粒界、すなわち結晶粒表面のみにおける
Ｃｒを多く含むＣｒの偏析領域の存在のみならず、好ま
しくは結晶粒内でのＣｒの偏析領域をも含めてその偏析
領域の特に膜面方向に関する間隔が垂直磁気特性、特に
垂直方向の保磁力Ｈｃ工に大きな影響を与えることの究
明に基づいてなされたものである。The present invention is directed not only to the existence of Cr segregation regions containing a large amount of Cr at grain boundaries, that is, only on the grain surfaces, but also preferably to the presence of Cr segregation regions within the grains, particularly on film surfaces of the Cr segregation regions. This was done based on the investigation that the spacing in the direction has a great influence on the perpendicular magnetic properties, especially the coercive force Hc in the perpendicular direction.
すなわち、本発明においては、Ｃｏ−Ｃｒ系磁性膜を有
する垂直磁気記録媒体を構成するものであるが、特にそ
のＧｏ−Ｃｒ系磁性膜の膜面に沿う全方向に関してすな
わち等方的に隣り合うＣｒ偏析領域の各配置間隔の平均
的距離つまり偏析領域の平均配置周期が、３０Å〜３０
０人の範囲となる構成とする。That is, in the present invention, a perpendicular magnetic recording medium having a Co-Cr magnetic film is constructed, and in particular, in all directions along the film surface of the Go-Cr magnetic film, that is, isotropically adjacent The average distance between each arrangement interval of the Cr segregation regions, that is, the average arrangement period of the segregation regions is 30 Å to 30
The configuration will be within the range of 0 people.
つまり、Ｃｏ−Ｃｒ磁性膜の、その膜面方向についての
断面におけるＣｏ−Ｃｒ結晶粒表面に生じる或いは（及
び）結晶粒内に生じる膜面に沿う断面でのＣｒを多く含
むＣｒ偏析領域が、同−結晶粒内或いは（及び）他の結
晶粒を含んで隣合うＣｒ偏析領域との配置間隔の等方的
平均が３０Å〜３００人の範囲にあるように選定する。In other words, the Cr-rich Cr-rich Cr-segregation region that occurs on the Co--Cr crystal grain surface and/or within the crystal grain in the cross-section along the film surface of the Co--Cr magnetic film is - Selection is made so that the isotropic average spacing between adjacent Cr segregation regions within the same crystal grain or (and) including other crystal grains is in the range of 30 Å to 300 Å.
尚、このようなＣｏ−Ｃｒ膜の偏析構造、すなわちＣｒ
偏析領域の分布態様は、その磁性膜の作製に当たっての
スパッタリング、もくしは蒸着条件と共に、カーボンＣ
の添加とその添加量の選定によって容易、確実に制御で
きるものであることが究明され、実際には、これら条件
の設定によって平均偏析周期を３０Å〜３００人に選定
する０例えば、スパッタリングによって目的とするＣｏ
−Ｃｒ磁性膜を形成する場合にはＣの添加量は、Ｃｏ−
Ｃｒ１ｉ全体の組成において０．１〜０．３原子％の範
囲とし、磁性膜作製のスパッタリングはスパッタリング
処理槽内の初期到達真空度Ｐｉ、すなわち、スパッタリ
ング処理槽内所定のアルゴン圧に設定する以前の槽内の
真空度をＩ Ｘ １０−７〜５ Ｘ １０−” Ｔｏｒ
ｒとする。また、その後に槽内にアルゴンＡｒを供給し
て保持するＡｒ圧ＰＡ工を３〜１５ｍＴｏｒｒとする。It should be noted that the segregation structure of such a Co-Cr film, that is, Cr
The distribution mode of the segregation region is determined by the sputtering or evaporation conditions used to produce the magnetic film, as well as the carbon C
It has been found that this can be easily and reliably controlled by adding and selecting the amount of addition.Actually, by setting these conditions, the average segregation period can be selected from 30 Å to 300 Å.For example, sputtering can be used to Co
When forming a -Cr magnetic film, the amount of C added is Co-
The overall composition of Cr1i is in the range of 0.1 to 0.3 at. The degree of vacuum in the tank is I x 10-7~5 x 10-” Tor
Let it be r. Further, the Ar pressure PA process for supplying and maintaining argon into the tank after that is set to 3 to 15 mTorr.
更にスパッタリング時の基体温度Ｔｓ、すなわち磁性膜
を形成する被スパツタリング基体の温度Ｔｓを１２０℃
〜１８０℃好ましくは１４０℃〜 １６０℃とする。Furthermore, the substrate temperature Ts during sputtering, that is, the temperature Ts of the substrate to be sputtered on which the magnetic film is formed, is set to 120°C.
-180°C, preferably 140°C - 160°C.
上述したように、Ｃｏ−Ｃｒ磁性膜において、特にその
膜面方向に関するＣｒの偏析領域の平均偏析周期を、３
０Å〜３００人に選定するとき、第１図にその偏析領域
の平均配置周期と磁気特性、特に垂直方向の保磁力Ｏｃ
ｔと、飽和磁化Ｍｓの測定結果を示すように、 Ｈｃよ
と１ ｋＯｅを得ることができると共にＭｓの増加がは
かられる。第１図において、曲線＋１１がそのｔｔｃ↓
の測定結果を示すものであり、曲線（２）がＣｏ−Ｃｒ
磁性膜の飽和磁化Ｍｓを、このＣｏ −Ｃｒ磁性膜を構
成する磁性材全体と同組成の合金バルクの飽和磁化１’
ｌｓｓに対する比ＭＳ／ ＭＳＢとして測定した結果を
示したものである。Ｃｒの偏析領域の平均配置周期が３
００人を越えるとＨＣＩが１ ｋｏｅより可成り小さく
なって垂直磁気記録媒体としての特徴の効果を発揮し得
ないが、平均配置周期が小さくなるほど、ＨＣＩとＭｓ
の増加がはかられている。しかしながら、この周期が３
０人未満となると、超常磁性となることが原因と推定さ
るＨＣ上の急激な低下が生じてくるという不都合がある
。As mentioned above, in a Co-Cr magnetic film, the average segregation period of the Cr segregation region, especially in the direction of the film surface, is set to 3.
When selecting 0 to 300 people, Figure 1 shows the average arrangement period and magnetic properties of the segregation region, especially the perpendicular coercive force Oc.
As shown in the measurement results of t and saturation magnetization Ms, 1 kOe can be obtained with Hc and Ms can be increased. In Figure 1, the curve +11 is the ttc↓
The curve (2) shows the measurement results for Co-Cr.
The saturation magnetization Ms of the magnetic film is expressed as the saturation magnetization 1' of the alloy bulk having the same composition as the entire magnetic material constituting this Co-Cr magnetic film.
The results are shown as the ratio MS/MSB to lss. The average arrangement period of the Cr segregation region is 3
If the number exceeds 00, the HCI becomes considerably smaller than 1 koe, and the characteristics of a perpendicular magnetic recording medium cannot be exhibited. However, as the average arrangement period becomes smaller, the HCI and Ms
is expected to increase. However, this period is 3
If the number is less than 0, there will be a disadvantage that there will be a sudden drop in HC, which is presumed to be caused by superparamagnetism.
因みに前述した特開昭６０−２４６０１６号公報に開示
された磁気記録媒体では、カーボンＣを０．０１〜１．
０重量％（０，０５〜４原子％）添加するものではある
が、この場合、飽和磁化Ｍｓの増加がみられていないも
のであり、このことからもこの公開公報に開示の磁気記
録媒体ではＣの添加にもかかわらず、本発明の構成が生
じていないものであること、つまりＣの添加によってＣ
ｒ偏析の促進がなされず、Ｃｒ偏析領域の平均配置周期
が３０Å〜３００人になっていないことがわかる。Incidentally, in the magnetic recording medium disclosed in the above-mentioned Japanese Patent Application Laid-open No. 60-246016, carbon C is contained in an amount of 0.01 to 1.
0% by weight (0.05 to 4 atomic%) is added, but in this case no increase in saturation magnetization Ms is observed, and for this reason, the magnetic recording medium disclosed in this publication does not. Despite the addition of C, the structure of the present invention does not occur, that is, the addition of C
It can be seen that r segregation is not promoted and the average arrangement period of Cr segregation regions is not 30 Å to 300 Å.
更に、本発明による垂直磁気記録媒体を得るに当たって
スパッタ条件の選定と共にそのＣの添加量をＣｏ −Ｃ
ｒ膜全全体しての組成において、０．１〜０．３原子％
に選定すれば良いものであるが、これは０．１原子％未
満ではＣｒ偏析領域の配置周期が大きくなり過ぎ、０．
３原子％を超えると磁気特性の劣化が生じてくることを
認めたことに因る。第２図はそのカーボンＣの添加量と
Ｍｓとの関係の測定結果を示したものである。Furthermore, in obtaining the perpendicular magnetic recording medium according to the present invention, sputtering conditions are selected and the amount of C added is changed to Co-C.
0.1 to 0.3 atomic% in the overall composition of the r film
However, if it is less than 0.1 atomic %, the arrangement period of the Cr segregation region becomes too large;
This is because it was recognized that magnetic properties deteriorate when the content exceeds 3 atomic %. FIG. 2 shows the measurement results of the relationship between the amount of carbon C added and Ms.
また、Ｃｏ−Ｃｒ磁性膜のスパッタ条件において、初期
到達真空度ＰｉをＩ Ｘ １０” 〜５ Ｘ １Ｏ−７
Ｔｏｒｒとするのは、この値がこれより大きいと雰囲気
中の不純物混入が大となって最終的に得られたＣｏ−Ｃ
ｒ磁性膜の特性にばらつきや劣化を生じてくるものであ
ることを認めたことに因る。また、スパッタリング処理
槽内のＡｒ圧を３〜１５ｍＴｏｒｒとするのは、３ ｓ
＋Ｔｏｒｒ未満では安定な放電が得られにくいなどの不
都合が生じ、１５ｍＴｏｒｒを超えると、Ｃｒの偏析が
生じにクク、偏析周期が大となり過ぎること、及びＣ軸
配向の低下、更に膜全体が多孔質になることを認めたこ
とに因る。更にまた、スパッタリングに際しての基体温
度Ｔｓを１２０°Ｃ〜１８０℃、好ましくは１４０℃〜
１６０℃とするのは、基体温度Ｔｓが低過ぎるとＣｒの
結晶粒子内での偏析が生じにくくなり、余り高くなると
表面荒れが生じてくることを認めたことに因る。In addition, under the sputtering conditions for the Co-Cr magnetic film, the initial vacuum degree Pi is I x 10'' to 5 x 1O-7
Torr is used because if this value is larger than this, the amount of impurities in the atmosphere will increase and the final Co-C
This is due to the fact that it has been recognized that variations and deterioration occur in the characteristics of r-magnetic films. In addition, the Ar pressure in the sputtering treatment tank is set to 3 to 15 mTorr for 3 s.
If it is less than + Torr, there will be problems such as difficulty in obtaining stable discharge, and if it exceeds 15 mTorr, Cr segregation will occur, the segregation period will become too large, the C-axis orientation will decrease, and the entire film will become porous. This is due to the fact that it has been acknowledged that Furthermore, the substrate temperature Ts during sputtering is 120°C to 180°C, preferably 140°C to
The reason why the temperature is set at 160° C. is based on the recognition that if the substrate temperature Ts is too low, segregation of Cr within the crystal grains becomes difficult to occur, and if it is too high, surface roughness occurs.
板状、シート状、或いはテープ状等の磁気記録媒体を構
成する非磁性基体、例えばポリアミドフィルム、ポリイ
ミドフィルム等の上にスパッタリング或いは蒸着によっ
てＣｒが１２〜２９原子％含むＣ。Carbon containing 12 to 29 atom % of Cr by sputtering or vapor deposition onto a nonmagnetic substrate constituting a magnetic recording medium such as a plate, sheet, or tape, such as a polyamide film or a polyimide film.
−Ｃｒ磁性膜を作製する。-Produce a Cr magnetic film.
実施例１
厚さ１２μｍのポリイミドフィルム基体上に、スパッタ
リングによってＣｏ−Ｃｒ磁性膜を被着形成した。この
スパッタリングは、第３図にその路線的構成図を示すよ
うに、スパッタリング処理槽（１）内に、陽極（■２）
と、陰極すなわちターゲラ）（１３）とが配置され、陽
極（１２）側に被スパツタリング基体（１４）が配置さ
れる。この基体（１４）の配置部には、この基体（１４
）を所要の温度に加熱する加熱手段（図示せず）が配置
される。槽（１１には、排気口（１５）が設けられ、こ
れが排気手段、すなわち真空ポンプに開閉弁（１６）を
介して連結される。（１７）はアルゴンの供給口で、開
閉弁（１８）を介してアルゴン供給源に連結される。（
２０）は例えば周波数１３．５６ＭＨｚの高周波電源で
両電極（１２）及び（１３）間に高周波を供給する。こ
の構成において、ターゲット（１３）とし、Ｃｒ２２重
量％、残部ＣｏによるＣｏ −Ｃｒ合金を用いて基体（
１４）上に、Ｃ０−Ｃｒ磁性膜をスパッタリングによっ
て作製した。Example 1 A Co--Cr magnetic film was formed by sputtering on a polyimide film substrate having a thickness of 12 μm. This sputtering is carried out by placing an anode (■2) in the sputtering treatment tank (1), as shown in the schematic diagram in Figure 3.
and a cathode (target layer) (13), and a substrate to be sputtered (14) is placed on the anode (12) side. This base body (14) is placed in the placement part of this base body (14).
) heating means (not shown) are arranged to heat the material to the required temperature. The tank (11) is provided with an exhaust port (15), which is connected to an exhaust means, that is, a vacuum pump, via an on-off valve (16). (17) is an argon supply port, and an on-off valve (18) connected to an argon source via
20) is a high frequency power supply with a frequency of 13.56 MHz, for example, which supplies high frequency between the electrodes (12) and (13). In this configuration, the target (13) is a Co-Cr alloy consisting of 22% by weight Cr and the balance Co.
14) A C0-Cr magnetic film was formed on top by sputtering.
この場合、メインスパッタリング時の高周波パワーは１
５０Ｗとし、基体（１４）とターゲット（１３）との間
の距離ｄを６ｃｍとし、初期到達真空度Ｐｉを２〜３
Ｘ １０” Ｔｏｒｒとし、メインスパッタリング中の
Ａｒ圧ＰＡ？を４．１ｗＴｏｒｒとし、基体温度Ｔｓを
１４０℃及び１６０℃にそれぞれ選定してそれぞれ厚さ
約０．６μ僻のＣｏ −Ｃｒ系磁性膜による試料Ａ及び
Ｂを得た。ここに基体温度Ｔｓはメインスパッタリング
の放電直後に測定した値である。これら膜中のＣｒ量は
ＥＤＸ （エネルギー分散型Ｘ線分光値Ｗ）によって
測定したところ２３原子％であった。In this case, the high frequency power during main sputtering is 1
50 W, the distance d between the base (14) and the target (13) was 6 cm, and the initial vacuum degree Pi was 2 to 3.
X 10" Torr, the Ar pressure PA during main sputtering was 4.1 wTorr, and the substrate temperature Ts was selected to be 140°C and 160°C, respectively. Samples A and B were obtained.The substrate temperature Ts here is the value measured immediately after the discharge of main sputtering.The amount of Cr in these films was measured by EDX (energy dispersive X-ray spectroscopy W) and was 23 atoms. %Met.
比較例１
上記の実施例１と同様の方法によるがＧｏ−Ｃｒ膜のス
パッタリングにおける基体温度Ｔｓを９０℃として磁性
膜の作製を行って試料Ｃを得た。Comparative Example 1 Sample C was obtained by fabricating a magnetic film in the same manner as in Example 1 above, but with the substrate temperature Ts of 90° C. during sputtering of the Go-Cr film.
実施例２
実施例１と同様の方法によるも、スパッタリング時の基
体温度Ｔｓを１４０℃とし、初期到達真空度Ｐｉを１．
５〜３．ＯＸ １Ｏ−７Ｔｏｒｒとし、メインスパッタ
リング時の高周波パワー １５０Ｗとした。そして、こ
の条件下で、メインスパッタリング時のＡｒ圧ｐ＾ｒを
それぞれ１０ｍＴｏｒｒ及び４．ｌｏ＋Ｔｏｒｒとして
Ｇｏ −Ｃｒ磁性膜の作製を行いそれぞれ試料り及びＥ
を得た。Example 2 The same method as in Example 1 was used, but the substrate temperature Ts during sputtering was 140° C., and the initial vacuum degree Pi was 1.
5-3. OX was set at 1O-7 Torr, and the high frequency power during main sputtering was set at 150W. Under these conditions, the Ar pressure p^r during main sputtering was set to 10 mTorr and 4.0 mTorr, respectively. A Go-Cr magnetic film was prepared at lo+Torr, and samples were prepared and E
I got it.
比較例２
実施例２と同様の方法によるが、この場合Ａｒ圧ＰＡ工
を３０ｍＴｏｒｒとして磁性膜の形成を行って試料Ｆを
得た。Comparative Example 2 Sample F was obtained by forming a magnetic film in the same manner as in Example 2, except that the Ar pressure PA process was set at 30 mTorr.
実施例３
実施例１と同様の方法によって基体（１４）上に、Ｃｏ
−Ｃｒ系磁性膜の作製を行って試料Ｇを得た。この場合
基体温度Ｔｓ＝ １４０℃及び１２０℃とし、ターゲッ
ト（１３）としては、カーボンＣのペレットを１及び３
面積％をもってＣｏ−Ｃｒ系合金上に配置した。Example 3 Co was deposited on the substrate (14) by the same method as in Example 1.
Sample G was obtained by fabricating a -Cr-based magnetic film. In this case, the substrate temperature Ts = 140°C and 120°C, and the target (13) is carbon C pellets 1 and 3.
It was arranged on the Co-Cr alloy with area%.
各実施例及び比較例によって得た各試料Ａ−１の磁性膜
についてのＨＣＡをＶＳＭ法（試料振動型磁力計）によ
って測定した結果と、ＥＤＸ法（エネルギー分散型Ｘ線
分光）によって測定したＣｒ量と、５１ＭＳ法（２次イ
オン質量分析）によって測定したＣの添加量と、更にＣ
ｒ偏析領域の平均配置周期Ｆとを、スパッタリングの諸
条件と共に第４図の表に示す。また、各試料Ａ−１にお
いて、その基体（１４）を溶解除去し、アトムミリング
によって薄膜化し、王水の希釈液で５〜１０分間いわゆ
るＣｏ１Ｊソチ（ｒｉｃｈ）部をエツチングしてその偏
析構造をＴＥ？Ｉ （透過型電子顕微鏡）で観察した
。尚、この観察方法については、ジャパニーズ・ジャー
ナル・オブ・アプライド・フィジクスＶＯＬ２５． Ｎ
ｏ、８゜８月、 １９８６． ｐｐ、 Ｌ６６８−Ｌ
６７０に記録されているところである。そして、この観
察方法によって観察された各試料Ａ−１のＣｒ偏析の態
様を第５図Ａ〜■に模式的に示す。第５図において斜線
を付して示した部分がＣｒの偏析領域（５１）であり、
（５２）は特に他部に比し、Ｃｏが富んだＣｏリッチ部
である。The HCA of the magnetic film of each sample A-1 obtained in each example and comparative example was measured by the VSM method (sample vibrating magnetometer), and the Cr measured by the EDX method (energy dispersive X-ray spectroscopy). amount, the added amount of C measured by the 51MS method (secondary ion mass spectrometry), and the amount of C added.
The average arrangement period F of the r-segregation regions is shown in the table of FIG. 4 together with the sputtering conditions. In each sample A-1, the substrate (14) was dissolved and removed, made into a thin film by atom milling, and the so-called Co1J rich part was etched with a diluted aqua regia solution for 5 to 10 minutes to clarify its segregation structure. TE? I (transmission electron microscope). This observation method is described in Japanese Journal of Applied Physics VOL25. N
o, 8° August, 1986. pp, L668-L
670 is recorded here. The mode of Cr segregation in each sample A-1 observed by this observation method is schematically shown in FIGS. The shaded area in FIG. 5 is the Cr segregation region (51),
(52) is a Co-rich part that is particularly rich in Co compared to other parts.
また、第６図Ａ〜■はそれぞれ試料Ａ〜■の各試料の各
膜表面のＴＥＭ １０万倍写真図である。Moreover, FIGS. 6A to 6 are 100,000x TEM photographs of the surfaces of the respective films of samples A to 6, respectively.
第７図は試料Ｂの同様の膜断面の写真図でこれによれば
柱状粒子が膜と垂直方向に良く配列していることが分か
る。FIG. 7 is a photographic diagram of a similar cross-section of the membrane of sample B, and it can be seen that the columnar particles are well arranged in the direction perpendicular to the membrane.
尚、上述した例ではスパッタリングによってＣ０−Ｃｒ
系磁性膜の作製を行った場合であるが、成る場合は真空
蒸着法によってその形成を行うことができる。In addition, in the above example, C0-Cr is
This is a case where a system magnetic film is produced, but if it is, it can be formed by vacuum evaporation method.
本発明によれば、例えば試料Ａ及びＢを試料Ｃと比較す
ることによって明らかなように、Ｃｒ偏析領域の平均配
置周波数が、６００人のものに比し、ｏｃＬが約５０％
以上向上し、試料り及びＥが試料Ｆに比し約４５％向上
し、更にＣｏリッチ部が網目構造の試料Ｇのものは、Ｃ
ｒ偏析部が中心部に存在する試料Ｆに比しそのｆｉａｔ
は７６％以上向上している。According to the present invention, for example, as is clear by comparing samples A and B with sample C, the average arrangement frequency of the Cr segregation region is approximately 50% ocL compared to that of 600 people.
The sample G has improved by about 45% compared to sample F, and the Co-rich portion has a network structure.
Compared to sample F in which the r-segregation part is present in the center, its fiat
has improved by more than 76%.
このように本発明によれば、Ｃｒ偏析領域の平均配置周
波数の特定によって垂直磁気特性を効果的に向上させる
ことができたものである。As described above, according to the present invention, the perpendicular magnetic properties can be effectively improved by specifying the average arrangement frequency of the Cr segregation region.
第１図はＣｒ偏析領域の平均配置周期と磁気特性との関
係を測定した結果を示す図、第２図はカーボン添加量に
対する飽和磁化ＭＳの測定結果を示す図、第３図は本発
明による垂直磁気記録媒体を得るスパッタリング装置の
構成図、第４図は本発明の実施例及び比較例の各試料の
特性測定結果等を示す表口、第５図Ａ−１はそれぞれ各
試料のＣｒ偏析状態を示す模式図、第６図Ａ−１はそれ
ぞれ各試料の膜表面の顕微鏡写真図、第７図は１試料の
膜断面の顕微鏡写真図である。
（１１）はスパッタリング処理、（１４）は被スパツタ
リング基体である。Figure 1 is a diagram showing the results of measuring the relationship between the average arrangement period of Cr segregation regions and magnetic properties, Figure 2 is a diagram showing the measurement results of saturation magnetization MS with respect to the amount of carbon added, and Figure 3 is a diagram according to the present invention. A block diagram of a sputtering apparatus for producing a perpendicular magnetic recording medium, FIG. 4 is a front page showing the measurement results of the characteristics of each sample of Examples and Comparative Examples of the present invention, and FIG. 5 A-1 shows the Cr segregation of each sample. A schematic diagram showing the state, FIG. 6 A-1 is a microscopic photograph of the membrane surface of each sample, and FIG. 7 is a microscopic photograph of the membrane cross section of one sample. (11) is a sputtering process, and (14) is a substrate to be sputtered.
Claims (1)
置周期が３０Å〜３００Åとされたことを特徴とする垂
直磁気記録媒体。[Scope of Claim] A perpendicular magnetic recording medium comprising a Co--Cr based magnetic film, characterized in that the average arrangement period of Cr segregation regions in the direction along the film surface is 30 Å to 300 Å.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9055987A JP2508703B2 (en) | 1987-04-13 | 1987-04-13 | Perpendicular magnetic recording media |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9055987A JP2508703B2 (en) | 1987-04-13 | 1987-04-13 | Perpendicular magnetic recording media |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63255813A true JPS63255813A (en) | 1988-10-24 |
| JP2508703B2 JP2508703B2 (en) | 1996-06-19 |
Family
ID=14001771
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9055987A Expired - Fee Related JP2508703B2 (en) | 1987-04-13 | 1987-04-13 | Perpendicular magnetic recording media |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2508703B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5352501A (en) * | 1989-12-27 | 1994-10-04 | Mitsubishi Kasei Corporation | Longitudinal magnetic recording medium comprising a circumterentially textured disk substrate, chromium primer layer and a cobalt chromium magnetic alloy layer having a segregation structure |
-
1987
- 1987-04-13 JP JP9055987A patent/JP2508703B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5352501A (en) * | 1989-12-27 | 1994-10-04 | Mitsubishi Kasei Corporation | Longitudinal magnetic recording medium comprising a circumterentially textured disk substrate, chromium primer layer and a cobalt chromium magnetic alloy layer having a segregation structure |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2508703B2 (en) | 1996-06-19 |
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