JPH04221429A - Manufacture of magnetic recording medium - Google Patents
Manufacture of magnetic recording mediumInfo
- Publication number
- JPH04221429A JPH04221429A JP41262990A JP41262990A JPH04221429A JP H04221429 A JPH04221429 A JP H04221429A JP 41262990 A JP41262990 A JP 41262990A JP 41262990 A JP41262990 A JP 41262990A JP H04221429 A JPH04221429 A JP H04221429A
- Authority
- JP
- Japan
- Prior art keywords
- layer
- room temperature
- magnetic recording
- recording medium
- temperature
- 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 58
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims description 23
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 12
- 239000011651 chromium Substances 0.000 claims description 12
- 238000010030 laminating Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 239000011135 tin Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000000137 annealing Methods 0.000 description 36
- 238000004544 sputter deposition Methods 0.000 description 12
- 238000010586 diagram Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 5
- 229910000531 Co alloy Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000003302 ferromagnetic material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910000684 Cobalt-chrome Inorganic materials 0.000 description 1
- WAIPAZQMEIHHTJ-UHFFFAOYSA-N [Cr].[Co] Chemical compound [Cr].[Co] WAIPAZQMEIHHTJ-UHFFFAOYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000010952 cobalt-chrome Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、ハードディスク装置等
に使用される磁気記録媒体に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a magnetic recording medium used in hard disk drives and the like.
【０００２】0002
【従来の技術】近年、ハードディスク装置は大容量化、
小型化の傾向にあり、この種の装置に用いられる磁気記
録媒体には、より高い記録密度が要求されている。上述
した高記録密度を実現するために、金属薄膜を磁性体層
として有する磁気記録媒体が実用化に向けて研究されて
いる。この種の磁気記録媒体のうち、基板上にクロム非
磁性層を積層し、この上にコバルト合金強磁性層を積層
した二層構造の磁気記録媒体は、良好な保磁力を示すこ
とが第１１回日本応用磁気学会学術講演概要集（１９８
７年）第１８頁に記載されている。更に、ここでは、ス
パッタリングによる各膜積層の際、基板温度を上昇させ
ることによりさらに高い保磁力が得られることが指摘さ
れている。上記した二層構造の磁気記録媒体を実際に製
造する場合、スパッタリングの前工程に基板の予備加熱
を行って基板温度を上昇させ、この状態で、クロム非磁
性層及びコバルト合金強磁性層を基板上に積層している
。具体的に言えば、インライン型スパッタリング装置に
よる磁気記録媒体の製造工程においては、多数枚のディ
スク基板をパレットに装着してスパッタリングする工程
の前に、この多数枚のディスク基板をパレットごと予備
加熱している。しかし、前述したような予備加熱処理で
は所定の温度まで加熱し、しかも各基板の均一な温度分
布を得るためには長時間を要するという問題点がある。
また、スパッタリング中は各基板温度の正確な制御が困
難なため、製造された各磁気記録媒体の保磁力がばらつ
くという問題点がある。一方、第５１回応用磁気学会学
術講演予稿集（１９９０年秋季）２６ａ−ＭＤ−５には
、２５０℃に加熱した基板上にクロム層、その上にコバ
ルト合金強磁性層を形成した後、この積層体を適当な条
件でアニールすることにより磁気記録媒体を製造し、こ
れによって保磁力を向上させている。この方法は、保磁
力がアニール温度及びアニール時間に依存するとを利用
したものである。[Background Art] In recent years, hard disk drives have become larger in capacity.
There is a trend toward miniaturization, and higher recording density is required of the magnetic recording media used in this type of device. In order to achieve the above-mentioned high recording density, magnetic recording media having a metal thin film as a magnetic layer are being studied for practical use. Among these types of magnetic recording media, magnetic recording media with a two-layer structure, in which a chromium nonmagnetic layer is laminated on a substrate and a cobalt alloy ferromagnetic layer is laminated thereon, exhibit good coercive force. Collected summaries of the academic lectures of the Japanese Society of Applied Magnetics (198
7 years) described on page 18. Furthermore, it is pointed out here that even higher coercivity can be obtained by increasing the substrate temperature when laminating each film by sputtering. When actually manufacturing the above-mentioned two-layer magnetic recording medium, the substrate is preheated in the pre-sputtering process to raise the substrate temperature, and in this state, the chromium nonmagnetic layer and the cobalt alloy ferromagnetic layer are attached to the substrate. layered on top. Specifically, in the process of manufacturing magnetic recording media using in-line sputtering equipment, before the process of mounting a large number of disk substrates on a pallet and sputtering, the large number of disk substrates are preheated together with the pallet. ing. However, the preheating treatment as described above has a problem in that it takes a long time to heat the substrate to a predetermined temperature and to obtain a uniform temperature distribution on each substrate. Furthermore, since it is difficult to accurately control the temperature of each substrate during sputtering, there is a problem in that the coercive force of each manufactured magnetic recording medium varies. On the other hand, in Proceedings of the 51st Academic Lectures of the Japan Society of Applied Magnetics (Autumn 1990) 26a-MD-5, a chromium layer is formed on a substrate heated to 250°C, and a cobalt alloy ferromagnetic layer is formed thereon. A magnetic recording medium is manufactured by annealing the laminate under appropriate conditions, thereby improving the coercive force. This method utilizes the fact that coercive force depends on annealing temperature and annealing time.
【０００３】0003
【発明が解決しようとする課題】しかし、上述した熱処
理のように、アニール温度及びアニール時間を定めただ
けでは、製造された磁気記録媒体の保磁力がばらつくこ
とが判明した。更に、上記した金属薄膜を磁性体層とす
る磁気記録媒体は主に二層構造のものに限られており、
多層構造のものについては考慮されていないのが実情で
ある。本発明の課題は、高い保磁力を有するとともに、
ばらつきが少なく、したがって、再現性の高い磁気記録
媒体の製造方法を提供することである。本発明の他の課
題は多層構造にしても、高い保磁力を得ることができる
磁気記録媒体の製造方法を提供することである。However, it has been found that simply setting the annealing temperature and annealing time as in the heat treatment described above causes variations in the coercive force of the manufactured magnetic recording media. Furthermore, magnetic recording media using the above-mentioned metal thin film as a magnetic layer are mainly limited to those with a two-layer structure.
The reality is that multilayer structures are not taken into account. The object of the present invention is to have high coercive force and
It is an object of the present invention to provide a method for manufacturing a magnetic recording medium with little variation and therefore high reproducibility. Another object of the present invention is to provide a method for manufacturing a magnetic recording medium that can obtain a high coercive force even if it has a multilayer structure.
【０００４】0004
【課題を解決するための手段】本発明の一態様によれば
、第１の工程で基板上に常温にて非磁性体である金属か
ら成る第１の層を室温乃至２００℃で積層し、第２の工
程で前記第１の層上に常温にて強磁性体である金属から
成る第２の層を室温乃至２００℃で常温下で積層して積
層体を製造し、つづいて第３の工程で前記積層体を常温
から３００℃以上まで所定の昇温速度で昇温し、第４の
工程で前記積層体を３００℃以上で所定の時間熱処理す
ることによって二層構造を有する磁気記録媒体の製造方
法が得られる。更に、本発明の他の態様によれば、第１
の工程で基板上に常温にて非磁性体である金属から成る
第１の層を室温乃至２００℃で積層し、第２の工程で前
記第１の層上に常温にて強磁性体である金属から成る第
２の層を室温乃至２００℃で積層し、第３の工程で前記
第２の層上に常温にて非磁性体である金属から成る第３
の層を室温乃至２００℃で積層して積層体を製造し、つ
づいて第４の工程で前記積層体を３００℃以上で所定の
時間熱処理することによって三層構造を有する磁気記録
媒体の製造方法が得られる。[Means for Solving the Problems] According to one aspect of the present invention, in a first step, a first layer made of a metal that is non-magnetic at room temperature is laminated on a substrate at room temperature to 200°C, In the second step, a second layer made of a metal that is ferromagnetic at room temperature is laminated on the first layer at room temperature to 200°C to produce a laminate, and then a third layer is formed. In the step, the temperature of the laminate is raised from room temperature to 300° C. or higher at a predetermined heating rate, and in the fourth step, the laminate is heat-treated at 300° C. or higher for a predetermined time, thereby producing a magnetic recording medium having a two-layer structure. A manufacturing method is obtained. Furthermore, according to another aspect of the invention, the first
In the step, a first layer made of a metal that is non-magnetic at room temperature is laminated on the substrate at room temperature to 200 ° C., and in the second step, a first layer made of a metal that is non-magnetic at room temperature is laminated on the first layer. A second layer made of metal is laminated at room temperature to 200°C, and in a third step, a third layer made of metal that is non-magnetic at room temperature is laminated on the second layer.
A method for producing a magnetic recording medium having a three-layer structure by laminating the layers at room temperature to 200°C to produce a laminate, and then heat-treating the laminate at 300°C or higher for a predetermined time in a fourth step. is obtained.
【０００５】[0005]
【作用】本発明では、基板上に常温にて非磁性体である
金属から成る第１の層を室温乃至２００℃で積層し、第
１の層上に常温にて強磁性体である金属から成る第２の
層を室温乃至２００℃で積層して積層体を製造し、つづ
いて前記積層体を常温から３００℃以上まで所定の昇温
速度で昇温し、所定の時間熱処理しているので、第１の
層の非磁性体が第２の層の結晶粒界へ熱拡散し、強磁性
体の各粒子間の強い磁気的相互作用を断ち切ることがで
きる。また、第１および第２の層を積層する際の温度は
上記のように室温乃至２００℃が好ましく、更に好まし
くは室温乃至１００℃以下、もっと好ましいのは室温で
ある。他方、２００℃を越えると各基板の温度がばらつ
き、結果として、磁気特性がばらつくため好ましくない
。[Operation] In the present invention, a first layer made of a metal that is non-magnetic at room temperature is laminated on a substrate at room temperature to 200°C, and a layer made of a metal that is ferromagnetic at room temperature is laminated on the first layer. A laminate is manufactured by laminating the second layer consisting of the following layers at room temperature to 200°C, and then the laminate is heated from room temperature to 300°C or higher at a predetermined temperature increase rate and heat-treated for a predetermined time. , the nonmagnetic material in the first layer thermally diffuses to the grain boundaries in the second layer, thereby breaking off the strong magnetic interaction between each grain of the ferromagnetic material. Further, the temperature at which the first and second layers are laminated is preferably room temperature to 200° C., more preferably room temperature to 100° C. or less, and even more preferably room temperature. On the other hand, if it exceeds 200°C, the temperature of each substrate will vary, resulting in variations in magnetic properties, which is not preferable.
【０００６】[0006]
【実施例】以下、本発明の実施例について詳細に説明す
る。本発明の実施例に用いたスパッタリング装置（図示
せず）は、複数のターゲットを備えたスパッタリングを
行うスパッタリング室と、アニールを行うアニール室を
備えている。両室はバルブを備えたチューブで連通して
おり、ガラス基板を大気にさらすことなく両室間を移動
させることができる。また、両室はそれぞれ真空ポンプ
を備えている。以下、本発明の第１の実施例について説
明する。まず、ガラス基板を常温であるスパッタリング
室にセットした後、室内を真空度が３×１０−６Ｔｏｒ
ｒに到達するまで排気した。続いて、Ａｒガスを導入し
た。このときのＡｒガス圧は１×１０−２Ｔｏｒｒであ
った。ガラス基板上にスパッタリングによって第１の層
としてクロム非磁性体層を３５０Ａ／分の速度で３００
０Ａ積層し、この上に第２の層としてＣｏ６０−Ｎｉ３
２．５−Ｃｒ７．５ 強磁性体層を３０Ａ／分の速度で
５００Ａ積層し、更に、この上に第３の層としてクロム
非磁性体層を３５０Ａ／分の速度で６０Ａ積層した。こ
のようにして、三層構造を有する第１の積層体ができた
。第１の積層体をアニール室に移動して、室内を真空度
が２×１０−５Ｔｏｒｒに到達するまで排気した。この
状態で種々の温度条件にてアニールを行い、磁気記録媒
体を製造した。製造された第１の磁気記録媒体の磁気特
性を、試料振動型磁力計を用いて測定した。測定結果を
図１乃至図３に示す。各図中の数字は磁気記録媒体の保
磁力（Ｏｅ）を表している。図１はアニール温度とアニ
ール時間を変化させたときの保磁力の値を示す。図１よ
りアニール温度３００℃乃至６００℃、アニール時間１
５分乃至１０時間なる条件のとき、保磁力が１４４８（
Ｏｅ）乃至２３５１（Ｏｅ）となり、保磁力向上に効果
的であることが分かる。なかでもアニール温度４００℃
乃至５００℃、アニール時間１時間乃至５時間のときが
、保磁力が２０００（Ｏｅ）以上となり特に効果的であ
る。図２はアニール温度と昇温速度を変化させたときの
保磁力の値を示す。図２より昇温速度が１℃／分乃至４
０℃／分のとき、保磁力が１６８３（Ｏｅ）乃至２３５
１（Ｏｅ）となり、保磁力向上に効果的であることが分
かる。
また、昇温速度が４０℃／分を越えると、保磁力向上効
果の減少に加えて、第１の層が剥離し易いため好ましく
ない。図３はアニール温度と降温速度を変化させたとき
の保磁力の値を示す。図３より降温速度が３０℃／時間
以上のとき、保磁力が１５０８（Ｏｅ）乃至２４０８（
Ｏｅ）となり、保磁力向上に効果的であることが分かる
。[Examples] Examples of the present invention will be described in detail below. The sputtering apparatus (not shown) used in the embodiment of the present invention includes a sputtering chamber that includes a plurality of targets and performs sputtering, and an annealing chamber that performs annealing. Both chambers are connected by a tube equipped with a valve, and the glass substrate can be moved between the two chambers without exposing it to the atmosphere. Additionally, both chambers are each equipped with a vacuum pump. A first embodiment of the present invention will be described below. First, after setting the glass substrate in a sputtering chamber at room temperature, the vacuum level in the chamber is set to 3 x 10-6 Torr.
It was evacuated until it reached r. Subsequently, Ar gas was introduced. The Ar gas pressure at this time was 1×10 −2 Torr. A chromium non-magnetic layer was deposited as a first layer on a glass substrate by sputtering at a rate of 300 A/min.
0A laminated, and Co60-Ni3 as a second layer on top of this.
A 2.5-Cr7.5 ferromagnetic layer was laminated at a rate of 30 A/min for 500 A, and a chromium nonmagnetic layer was further laminated thereon for 60 A at a rate of 350 A/min as a third layer. In this way, a first laminate having a three-layer structure was produced. The first laminate was moved to an annealing chamber, and the chamber was evacuated until the degree of vacuum reached 2×10 −5 Torr. In this state, annealing was performed under various temperature conditions to produce magnetic recording media. The magnetic properties of the manufactured first magnetic recording medium were measured using a sample vibrating magnetometer. The measurement results are shown in FIGS. 1 to 3. The numbers in each figure represent the coercive force (Oe) of the magnetic recording medium. FIG. 1 shows the values of coercive force when annealing temperature and annealing time are varied. From Figure 1, the annealing temperature is 300°C to 600°C, and the annealing time is 1.
Under conditions of 5 minutes to 10 hours, the coercive force is 1448 (
Oe) to 2351 (Oe), which shows that it is effective in improving coercive force. Among them, the annealing temperature is 400℃
When the temperature is 500° C. and the annealing time is 1 hour to 5 hours, the coercive force becomes 2000 (Oe) or more, which is particularly effective. FIG. 2 shows the values of coercive force when the annealing temperature and heating rate were varied. From Figure 2, the temperature increase rate is 1°C/min to 4°C.
At 0℃/min, the coercive force is 1683 (Oe) to 235
1 (Oe), which shows that it is effective in improving coercive force. Moreover, if the temperature increase rate exceeds 40° C./min, the effect of improving coercive force is reduced and the first layer is likely to peel off, which is not preferable. FIG. 3 shows the values of coercive force when the annealing temperature and cooling rate were varied. From Figure 3, when the temperature decreasing rate is 30°C/hour or more, the coercive force is 1508 (Oe) to 2408 (Oe).
Oe), which shows that it is effective in improving coercive force.
【０００７】次に、第１の実施例と同じ装置を用いて行
った第２の実施例を説明する。まず、ガラス基板を常温
であるスパッタリング室にセットした後、室内を真空度
が３×１０−６Ｔｏｒｒに到達するまで排気した。続い
て、Ａｒガスを導入した。このときのＡｒガス圧は１×
１０−２Ｔｏｒｒであった。ガラス基板上にスパッタリ
ングによって第１の層としてクロム非磁性体層を３５０
Ａ／分の速度で３０００Ａ積層し、この上に第２の層と
してＣｏ６０−Ｎｉ３２．５−Ｃｒ７．５ 強磁性体層
を３０Ａ／分の速度で厚さ５００Ａ積層した。このよう
にして、二層構造を有する第２の積層体ができた。次に
、第２の積層体をアニール室に移動して、室内を真空度
が２×１０−５Ｔｏｒｒに到達するまで排気した。この
状態で種々の温度条件にてアニールを行い、第２の磁気
記録媒体を製造した。製造された第２の磁気記録媒体の
磁気特性を、試料振動型磁力計を用いて測定したところ
、第１の実施例と同様の結果が得られた。図４はアニー
ル温度と昇温速度を変化させたときの保磁力の値を示す
。図４より昇温速度が１℃／分乃至４０℃／分のとき、
保磁力が１２０２（Ｏｅ）乃至１８２１（Ｏｅ）となり
、保磁力向上に効果的であることが分かる。また、昇温
速度が４０℃／分を越えると、保磁力向上効果の減少に
加えて、第１の層が剥離し易いため好ましくない。図５
はアニール温度を変化させたときの保磁力の値を示す。
尚、このときのアニール時間はいずれも３０分である。
図５よりアニール温度３００℃乃至６００℃のときが、
保磁力向上に効果的であることが分る。図６はアニール
温度を４００℃に保ち、アニール時間を変化させたとき
の保磁力の値を示す。図６よりアニール時間１５分乃至
１０時間のときが、保磁力向上に効果的であることが分
かる。Next, a second embodiment using the same apparatus as the first embodiment will be described. First, a glass substrate was set in a sputtering chamber at room temperature, and then the chamber was evacuated until the degree of vacuum reached 3×10 −6 Torr. Subsequently, Ar gas was introduced. At this time, the Ar gas pressure is 1×
It was 10-2 Torr. A chromium nonmagnetic layer with a thickness of 350 nm is deposited as a first layer on a glass substrate by sputtering.
A layer of 3000 A was laminated at a rate of A/min, and a Co60-Ni32.5-Cr7.5 ferromagnetic layer was laminated thereon to a thickness of 500 A at a rate of 30 A/min as a second layer. In this way, a second laminate having a two-layer structure was created. Next, the second laminate was moved to an annealing chamber, and the chamber was evacuated until the degree of vacuum reached 2×10 −5 Torr. In this state, annealing was performed under various temperature conditions to produce a second magnetic recording medium. When the magnetic properties of the manufactured second magnetic recording medium were measured using a sample vibrating magnetometer, results similar to those of the first example were obtained. FIG. 4 shows the values of coercive force when the annealing temperature and heating rate were changed. From Figure 4, when the temperature increase rate is 1°C/min to 40°C/min,
It can be seen that the coercive force is 1202 (Oe) to 1821 (Oe), which is effective in improving the coercive force. Moreover, if the temperature increase rate exceeds 40° C./min, the effect of improving coercive force is reduced and the first layer is likely to peel off, which is not preferable. Figure 5
indicates the value of coercive force when the annealing temperature is changed. Note that the annealing time at this time was 30 minutes. From Figure 5, when the annealing temperature is 300°C to 600°C,
It is found that this is effective in improving coercive force. FIG. 6 shows the coercive force values when the annealing temperature was maintained at 400° C. and the annealing time was varied. It can be seen from FIG. 6 that an annealing time of 15 minutes to 10 hours is effective in improving the coercive force.
【０００８】第１及び第２の実施例におけるアニールに
よる保磁力向上の原因を調べるために各磁気記録媒体を
ＴＥＭによって観察した。第２の層である強磁性体層中
の結晶粒径は５００Ａ乃至１０００Ａであった。また、
ＴＥＭ微小領域分析によりこの層中の結晶粒界のクロム
濃度が約３５ａｔ％と、結晶粒内のクロム濃度７．５ａ
ｔ％に比べて明らかに高いことが定量的に確認できた。
このことから、アニールによって強磁性体層中に拡散し
た非磁性体であるクロムが、各強磁性体結晶粒の周囲を
包囲したことが分かる。更に、上述した結晶粒界のクロ
ム濃度（約３５ａｔ％）が強磁性体であるコバルト合金
を非磁性化できることをコバルト−クロム系の平衡状態
図より確認した。このことから、非磁性体が強磁性体層
中に拡散することによって、各結晶粒間に存在していた
強い磁気的相互作用が断ち切られ各結晶粒が磁気的に孤
立するため、高い保磁力が得られると考えられる。In order to investigate the cause of the improvement in coercive force due to annealing in the first and second embodiments, each magnetic recording medium was observed using a TEM. The crystal grain size in the ferromagnetic layer, which is the second layer, was 500A to 1000A. Also,
TEM micro-area analysis shows that the chromium concentration at the grain boundaries in this layer is approximately 35 at%, and the chromium concentration within the grains is 7.5 at%.
It was quantitatively confirmed that it was clearly higher than t%. This shows that chromium, which is a nonmagnetic substance, diffused into the ferromagnetic layer by annealing and surrounded each ferromagnetic crystal grain. Furthermore, it was confirmed from the cobalt-chromium system equilibrium diagram that the above-mentioned chromium concentration (approximately 35 at %) at the grain boundaries can make a ferromagnetic cobalt alloy nonmagnetic. From this, when the nonmagnetic material diffuses into the ferromagnetic material layer, the strong magnetic interaction that existed between each crystal grain is severed and each crystal grain becomes magnetically isolated, resulting in a high coercive force. is considered to be obtained.
【０００９】尚、上記実施例における第１及び第３の層
の非磁性体から成る金属としては、例えば、クロム、ケ
イ素、アルミニウム、チタン、ビスマス、バナジウム、
マンガン、錫、亜鉛、ゲルマニウム、鉛、インジウム、
銅、モリブデン、タングステンの内から選ばれた少なく
とも１つであればよい。また、第２の層の強磁性体から
成る金属としては、コバルト、ニッケル、鉄の内から選
ばれた少なくとも１つであればよい。更に、アニールの
際の雰囲気はアルゴン、窒素、及び大気等でもよい。[0009] In the above embodiment, examples of the non-magnetic metal of the first and third layers include chromium, silicon, aluminum, titanium, bismuth, vanadium,
Manganese, tin, zinc, germanium, lead, indium,
It may be at least one selected from copper, molybdenum, and tungsten. Further, the metal of the ferromagnetic material of the second layer may be at least one selected from cobalt, nickel, and iron. Furthermore, the atmosphere during annealing may be argon, nitrogen, air, or the like.
【００１０】0010
【発明の効果】本発明によれば、基板上に非磁性体層及
び強磁性体層とが積層された積層体を製造した後、常温
から３００℃以上まで所定の昇温速度で昇温し、所定の
時間熱処理しているから、高い保磁力を有するとともに
、ばらつきが少なく、したがって、再現性の高い磁気記
録媒体を製造することができる。According to the present invention, after manufacturing a laminate in which a nonmagnetic layer and a ferromagnetic layer are laminated on a substrate, the temperature is increased from room temperature to 300° C. or higher at a predetermined heating rate. Since the magnetic recording medium is heat-treated for a predetermined period of time, it is possible to manufacture a magnetic recording medium that has a high coercive force and has little variation, and therefore has high reproducibility.
【図１】アニール温度及びアニール時間と磁気記録媒体
の保磁力との関係を示す図である。FIG. 1 is a diagram showing the relationship between annealing temperature, annealing time, and coercive force of a magnetic recording medium.
【図２】アニール温度及び昇温速度と磁気記録媒体の保
磁力との関係を示す図である。FIG. 2 is a diagram showing the relationship between annealing temperature, temperature increase rate, and coercive force of a magnetic recording medium.
【図３】アニール温度及び降温速度と磁気記録媒体の保
磁力との関係を示す図である。FIG. 3 is a diagram showing the relationship between the annealing temperature and temperature decreasing rate and the coercive force of the magnetic recording medium.
【図４】アニール温度及び昇温速度と磁気記録媒体の保
磁力との関係を示す図である。FIG. 4 is a diagram showing the relationship between annealing temperature, temperature increase rate, and coercive force of a magnetic recording medium.
【図５】アニール温度と磁気記録媒体の保磁力との関係
を示す図である。FIG. 5 is a diagram showing the relationship between annealing temperature and coercive force of a magnetic recording medium.
【図６】アニール時間と磁気記録媒体の保磁力との関係
を示す図である。FIG. 6 is a diagram showing the relationship between annealing time and coercive force of a magnetic recording medium.
Claims (4)
から成る第１の層を積層する第１の工程と、前記第１の
層上に常温にて強磁性体である金属から成る第２の層を
積層する第２の工程と、前記第２の層上に常温にて非磁
性体である金属から成る第３の層を積層する第３の工程
とを含み、前記第１、第２及び第３の工程を室温乃至２
００℃で行って積層体を製造する工程につづいて、前記
積層体を常温から３００℃以上まで所定の昇温速度で昇
温する第４の工程と、前記積層体を３００℃以上で所定
の時間熱処理する第５の工程とを含むことを特徴とする
磁気記録媒体の製造方法。1. A first step of laminating a first layer made of a metal that is non-magnetic at room temperature on a substrate, and a step of laminating a first layer made of a metal that is ferromagnetic at room temperature on the first layer. a second step of laminating a second layer; a third step of laminating a third layer made of a metal that is non-magnetic at room temperature on the second layer; The second and third steps are carried out at room temperature
Following the step of manufacturing the laminate at 00°C, a fourth step of raising the temperature of the laminate from room temperature to 300°C or higher at a predetermined temperature increase rate, and heating the laminate at 300°C or higher at a predetermined temperature increase rate. A method for manufacturing a magnetic recording medium, comprising a fifth step of performing heat treatment for a period of time.
４０℃／分であることを特徴とする請求項１記載の磁気
記録媒体の製造方法。2. The method of manufacturing a magnetic recording medium according to claim 1, wherein the predetermined temperature increase rate is from 1° C./min to 40° C./min.
とも一方が、クロム、ケイ素、アルミニウム、チタン、
ビスマス、バナジウム、マンガン、錫、亜鉛、ゲルマニ
ウム、鉛、インジウム、銅、モリブデン、タングステン
のグループから選ばれた少なくとも１つの非磁性体であ
る金属から成り、前記第２の層がコバルト、ニッケル、
鉄のグループから選ばれた少なくとも１つの強磁性体で
ある金属から成ることを特徴とする請求項１または２記
載の磁気記録媒体の製造方法。3. At least one of the first and third layers comprises chromium, silicon, aluminum, titanium,
The second layer is made of at least one non-magnetic metal selected from the group consisting of bismuth, vanadium, manganese, tin, zinc, germanium, lead, indium, copper, molybdenum, and tungsten, and the second layer is made of cobalt, nickel,
3. The method of manufacturing a magnetic recording medium according to claim 1, wherein the magnetic recording medium is made of at least one ferromagnetic metal selected from the iron group.
から成る第１の層を積層する第１の工程と、前記第１の
層上に常温にて強磁性体である金属から成る第２の層を
積層する第２の工程とを含み、前記第１及び第２の工程
を室温乃至２００℃で行って積層体を製造する工程につ
づいて、前記積層体を常温から３００℃以上まで所定の
昇温速度で昇温する第３の工程と、前記積層体を３００
℃以上で所定の時間熱処理する第４の工程とを含むこと
を特徴とする磁気記録媒体の製造方法。4. A first step of laminating a first layer made of a metal that is non-magnetic at room temperature on a substrate; and a first step of laminating a first layer made of a metal that is ferromagnetic at room temperature on the first layer. a second step of laminating a second layer, and following a step of manufacturing a laminate by performing the first and second steps at room temperature to 200°C, the laminate is laminated from room temperature to 300°C or higher; a third step of heating the laminate at a predetermined heating rate until 300 ml.
A method for manufacturing a magnetic recording medium, comprising a fourth step of heat-treating at a temperature of .degree. C. or higher for a predetermined period of time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2412629A JP2720363B2 (en) | 1990-12-21 | 1990-12-21 | Manufacturing method of magnetic recording medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2412629A JP2720363B2 (en) | 1990-12-21 | 1990-12-21 | Manufacturing method of magnetic recording medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04221429A true JPH04221429A (en) | 1992-08-11 |
| JP2720363B2 JP2720363B2 (en) | 1998-03-04 |
Family
ID=18521446
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2412629A Expired - Lifetime JP2720363B2 (en) | 1990-12-21 | 1990-12-21 | Manufacturing method of magnetic recording medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2720363B2 (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5670618A (en) * | 1979-11-15 | 1981-06-12 | Matsushita Electric Ind Co Ltd | Manufacture of cobalt chrome alloy thin film |
| JPS5877024A (en) * | 1981-10-29 | 1983-05-10 | Tdk Corp | Magnetic recording medium |
| JPH01186484A (en) * | 1988-01-21 | 1989-07-25 | Nippon Telegr & Teleph Corp <Ntt> | Inside-pipe self-traveling device |
| JPH0267897A (en) * | 1988-09-02 | 1990-03-07 | Fujitsu Ltd | Service control system in exchange |
| JPH02292715A (en) * | 1989-05-02 | 1990-12-04 | Hitachi Metals Ltd | Magnetic recording medium and its production |
-
1990
- 1990-12-21 JP JP2412629A patent/JP2720363B2/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5670618A (en) * | 1979-11-15 | 1981-06-12 | Matsushita Electric Ind Co Ltd | Manufacture of cobalt chrome alloy thin film |
| JPS5877024A (en) * | 1981-10-29 | 1983-05-10 | Tdk Corp | Magnetic recording medium |
| JPH01186484A (en) * | 1988-01-21 | 1989-07-25 | Nippon Telegr & Teleph Corp <Ntt> | Inside-pipe self-traveling device |
| JPH0267897A (en) * | 1988-09-02 | 1990-03-07 | Fujitsu Ltd | Service control system in exchange |
| JPH02292715A (en) * | 1989-05-02 | 1990-12-04 | Hitachi Metals Ltd | Magnetic recording medium and its production |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2720363B2 (en) | 1998-03-04 |
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