JPS6028028A - Production of magnetic recording medium - Google Patents

Production of magnetic recording medium

Info

Publication number
JPS6028028A
JPS6028028A JP13442583A JP13442583A JPS6028028A JP S6028028 A JPS6028028 A JP S6028028A JP 13442583 A JP13442583 A JP 13442583A JP 13442583 A JP13442583 A JP 13442583A JP S6028028 A JPS6028028 A JP S6028028A
Authority
JP
Japan
Prior art keywords
iron
ionized
ion
electrode
recording medium
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
Application number
JP13442583A
Other languages
Japanese (ja)
Other versions
JPH0334621B2 (en
Inventor
Tetsuo Tatsuno
龍野 哲男
Setsu Arikawa
有川 節
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taiyo Yuden Co Ltd
Original Assignee
Taiyo Yuden Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Taiyo Yuden Co Ltd filed Critical Taiyo Yuden Co Ltd
Priority to JP13442583A priority Critical patent/JPS6028028A/en
Publication of JPS6028028A publication Critical patent/JPS6028028A/en
Publication of JPH0334621B2 publication Critical patent/JPH0334621B2/ja
Granted legal-status Critical Current

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Landscapes

  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Thin Magnetic Films (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

PURPOSE:To obtain a magnetic recording medium having high coercive force and high durability by vapor depositing an iron molecule which is ionized by a rate higher than a specific% as well as iron and iron nitride to the surface of a nonmagnetic substrate at a specific incident angle after ionizing N higher than a specific% to the iron and an iron ion. CONSTITUTION:A crucible 2 containing iron 1 of 99.9% purity is used together with an electron beam irradiation source 3 for the iron 1, a radiation filament 4 for ionizing thermion of iron molecule, an ionizing electrode 5, an ion collecting electrode 6 for measurement of iron ion and nitrogen ion, a film thickness meter 7, and an ion gun 9 for ionization and iron acceleration of N2 gas flowed from a valve 8. A substrate 10 of glass, etc. is set on the electrode 6 so as to secure a >=50 deg. incident angle to the surface of the substrate, and a positive potential is applied to the electrode 5. Then the vapor deposition is carried out under the conditions where >=5% ionized iron exists to the sum of iron and ionized iron and N is ionized within a 5-100% range of the sum of the iron and the ionized iron. Thus it is possible to obtain a recording medium which excels in acid resistance and wear resistance. In addition, the lifetime of the filament 4 is also increased.

Description

【発明の詳細な説明】 本発明は、非磁性基材面に高保磁力を有する磁性薄膜を
被着形成する磁気記録媒体の製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing a magnetic recording medium in which a magnetic thin film having a high coercive force is deposited on the surface of a nonmagnetic base material.

近年、長時間録画や8%ビデオ用等のテープの小型化等
の要求に応えうる高密度磁気記録媒体として金属磁性薄
膜の秀れた磁気特性が注目されている。従来、このよう
な磁性金属薄膜材料としてコバルト又はコバルト・ニッ
ケル合金が利用されていたが、これ等の磁性薄膜社耐酸
化性や耐摩耗性が劣る欠点があった。
In recent years, the excellent magnetic properties of metal magnetic thin films have attracted attention as high-density magnetic recording media that can meet the demands for miniaturization of tapes for long-time recording, 8% video, and the like. Conventionally, cobalt or cobalt-nickel alloys have been used as such magnetic metal thin film materials, but these magnetic thin films have the drawback of poor oxidation resistance and wear resistance.

そこで本出願人は、これ等の特性が優れた磁性材料とし
て知られている窒化鉄に着目し、これ等の特性を有する
とともに保磁力が少なくとも600エルステツドの鉄及
び窒化鉄からなる磁性薄膜の製造方法を提案した(fr
uit昭57−197149゜ この方法は% 10−” Torr以下の窒素ガス中で
鉄蒸気を108以上イオン化しくイオン化率η)、該窒
素ガスを鉄及び鉄イオンに対して5〜50%イオン化し
、非磁性基材面に対し50度以上の入射角で斜方入射蒸
着をするものであるが、成膜速度を上げたとき、被蒸着
面に飛来する窒素イオンと鉄及び鉄イオンとの相対比率
(ξ)が減少し、磁性薄膜の保磁力れ著しく減少する。
Therefore, the present applicant focused on iron nitride, which is known as a magnetic material with excellent properties, and developed a magnetic thin film made of iron and iron nitride that has these properties and has a coercive force of at least 600 oersteds. proposed a method (fr
uit 1971-149゜This method ionizes iron vapor to 108 or more in nitrogen gas of % 10-'' Torr or less (ionization rate η), and ionizes the nitrogen gas to 5 to 50% of iron and iron ions, Oblique incidence deposition is performed at an incident angle of 50 degrees or more with respect to the non-magnetic base material surface, but when the deposition rate is increased, the relative ratio of nitrogen ions and iron and iron ions that fly to the deposition surface (ξ) decreases, and the coercive force of the magnetic thin film decreases significantly.

該相対比率を一定に・保つために成膜速度に対応させて
窒素ガス圧を高((10−3Torr以上)しても、鉄
及び鉄イオンの平均自由行程が短くなり、直進性が失わ
れて入射角が分散し、衣1の保磁力特性(単位エルステ
ッド)に示すように成膜速度νが速いところでは所期の
保磁力(例えば600エルステツド)が得られず%tf
c鉄蒸発用電子ビーム用フィラメントの寿命が極端に短
くなると共に該フイラメンFの近傍で異常放電が発生し
やすい不都合が生じた。
Even if the nitrogen gas pressure is increased (10-3 Torr or higher) in accordance with the film formation rate in order to keep the relative ratio constant, the mean free path of iron and iron ions becomes shorter and straightness is lost. As shown in the coercive force characteristics (unit: Oersteds) of coating 1, the desired coercive force (for example, 600 Oersteds) cannot be obtained when the film formation rate ν is high, and %tf
(c) The life of the electron beam filament for iron evaporation was extremely shortened, and abnormal discharge was likely to occur in the vicinity of the filament F.

表 1 (単位エルステッド) 以下本発明の実施例を図面につき説明する。Table 1 (Unit: Oersted) Embodiments of the present invention will be described below with reference to the drawings.

本発明の製造方法を実施するためrcrjA面に示すよ
うな装置を使用した。
In order to carry out the manufacturing method of the present invention, an apparatus as shown in the rcrjA side was used.

を収容したるつぼ(2)と該鉄(1)に対し電子ビーム
を照射してこれを蒸発させる電子ビーム放射源(3)と
鉄蒸気をイオン化するための熱電子放射フィラメント(
4)及びイオン化vL視(5)と、鉄イオン及び窒素イ
オン数を計かすするためのイオン捕集用電極(6)と、
膜厚計(7)と、パルプ(8)を介して流入する窒素ガ
スをイオン化すると共に該窒素イオンを加速する例えば
フリーマン型イオン銃(9)とから成り、例えばI O
’−’Torrに減圧された兵窒檜(図示せず)内に配
置した。
a crucible (2) containing iron, an electron beam radiation source (3) that irradiates the iron (1) with an electron beam to evaporate it, and a thermionic emission filament (3) that ionizes the iron vapor.
4) and ionization VL viewing (5), and an ion collection electrode (6) for counting the number of iron ions and nitrogen ions;
It consists of a film thickness meter (7) and, for example, a Freeman type ion gun (9) that ionizes nitrogen gas flowing through the pulp (8) and accelerates the nitrogen ions, such as an I O
It was placed in a Hyonitsu cypress (not shown) which was evacuated to '-' Torr.

鉄及び窒化鉄を蒸着する被着基材例えばガラス板(イ)
を板面が入射角θが50度になるようにイオン捕集用電
極(6)上に!置した。
Substrate to which iron and iron nitride are deposited, such as a glass plate (a)
on the ion collection electrode (6) so that the plate surface has an incident angle θ of 50 degrees! I placed it.

先ず^空槽内をI O”−’Torr 4C減圧し、鉄
(1)に電子ビームを照射して蒸発させ、膜厚計(7)
によp測定した成膜速度νが所定の速度例えはlO〜−
となるように電子ビーム放射源(3)の出力を詭整し1
次に熱電子放射フィラメント(4)に通電すると共にイ
オン化電極(6)ニ正電位を印加してイオン捕集用電極
(6)に流れる電流から1秒当j)lal&に飛来する
鉄イオン数tを測定し、t=4XlO”個/ ai 、
 amすなわち前記成膜速度から換算した鉄及び鉄イオ
ン数置= 8 X 101’個/ d 、 wcK対し
て−となるようにイオン化電極(5)の正電位を設Zt
) 定して鉄及び鉄イオン数に対する鉄のイオン化率ηを5
%とした。次にイオン銃(9)によ多窒素イオンをガラ
ス板01面に向けて照射し、このときイオン捕集用電極
(6)に流れる電流からめたイオン数が例えは12 X
 I O14個/ trA 、 scすなわち該イオン
数から前記tを減じて得た窒素イオン数n = 4 X
 l O”個の前記mに対する割合ξが5%となるよう
に窒素イオン照射量をm整した。
First, reduce the pressure in the empty tank to 4C to IO''-'Torr, irradiate the iron (1) with an electron beam to evaporate it, and measure the film thickness (7).
If the film formation rate ν measured by p is a predetermined rate, for example lO~-
Adjust the output of the electron beam radiation source (3) so that 1
Next, electricity is applied to the thermionic emission filament (4), and a positive potential is applied to the ionizing electrode (6), and the number of iron ions flying into the ion trapping electrode (6) per second is calculated from the current flowing to the ion collecting electrode (6). t=4XlO”/ai,
The positive potential of the ionization electrode (5) is set so that the number of iron and iron ions calculated from the film formation rate is -8 x 101' pieces/d, wcK, that is, Zt.
), and the iron ionization rate η for iron and the number of iron ions is 5.
%. Next, the ion gun (9) irradiates a large number of nitrogen ions toward the glass plate 01, and at this time, the number of ions collected from the current flowing through the ion collection electrode (6) is, for example, 12
IO14/trA, sc, i.e., the number of nitrogen ions obtained by subtracting the above t from the number of ions, n = 4 X
The amount of nitrogen ion irradiation was adjusted to m so that the ratio ξ of l O'' to the m was 5%.

以上のX空槽内の設定条件が安定したvk1ガラス板叫
を覆うシャッタを開いて100秒間蒸着し、膜厚が1o
oo;の薄膜を作成した。
The above setting conditions in the X-vacuum tank were stable.The shutter covering the VK1 glass plate was opened and vapor deposition was performed for 100 seconds until the film thickness was 10.
A thin film of oo; was created.

以上と同じ要領によシ成膜速度ν:10A/sc*20
 A / see 、 50^/m、10−0^/就及
び200λ/紅のそれぞれについて、入射角度0を50
度及び80度にして前記η:5%、10%。
Film formation speed ν: 10A/sc*20 in the same manner as above
For each of A/see, 50^/m, 10-0^/m, and 200λ/red, set the incident angle 0 to 50
and 80 degrees, said η: 5%, 10%.

20Xとξ:5N、10%、20%、50%。20X and ξ: 5N, 10%, 20%, 50%.

100Xとを組合せた条件で膜厚1000Aの薄膜を作
成した。
A thin film with a thickness of 1000A was created under the conditions of combining 100X and 100X.

そしてこれ等の薄J[4Cついて被着基材面に平行KI
Oキロエルステッドの外部磁界を印加して保磁力Hc 
を試料振動型磁力計によシ測定した。
Then, these thin J[4C KI parallel to the adherend substrate surface
By applying an external magnetic field of O kilo Oersted, the coercive force Hc
was measured using a sample vibrating magnetometer.

その結果を嚢2に示す。The results are shown in bag 2.

表2から明らかなように、ガラス板面に対し鉄の蒸気を
入射角50度の斜方から蒸着した場合において、鉄蒸気
klO,X及び2ONイオン化し。
As is clear from Table 2, when iron vapor was obliquely deposited onto the glass plate surface at an incident angle of 50 degrees, the iron vapor klO,X and 2ON were ionized.

イオン銃(9)からガラス板面に向けて鉄及び鉄イオン
に対する窒素イオンの割合ξを5%〜50%変化させて
窒素イオンを照射したとき、ξが5Xでは600〜63
0エルステツド、ξが10〜50Xでは690〜720
エルステツドの範囲の保磁力が成膜速度(10〜200
λ/(6))に関係なく得られた。
When nitrogen ions are irradiated from the ion gun (9) toward the glass plate surface by changing the ratio ξ of iron and nitrogen ions to iron ions by 5% to 50%, when ξ is 5X, it is 600 to 63.
0 oersted, 690-720 when ξ is 10-50X
The coercive force in the Oersted range increases the deposition rate (10 to 200
was obtained regardless of λ/(6)).

入射角を80度にした場合において、鉄蒸気を5%、1
0%及び20%イオン化し、ξを5〜100%変化させ
て窒素イオンを照射したときη:5%及びξ:5%では
810〜820エルステツド、η:596及びξ:lO
〜50%では940〜960エルステツド、η:10%
及ヒ20%並びにξ:5%では1000〜1030エル
ステッド、4210%及び20%並びに0210%〜5
0%では1230〜1250エルステツド、η:5%及
びξ二10ONでは780〜810エルステツド、η:
10X及び20%並びにξ:100Nで社900〜97
0エルステッドの範囲の保磁力が成膜速度(10〜20
0人/臓)に影響を受けずに得られた。
When the incident angle is 80 degrees, 5% iron vapor and 1
When nitrogen ions were irradiated with 0% and 20% ionization and ξ was varied from 5 to 100%, η: 5% and ξ: 5% resulted in 810 to 820 oersted, η: 596 and ξ: lO
~50% is 940-960 oersted, η: 10%
1000 to 1030 oersted for 20% and 5%, 4210% and 20% and 0210% to 5
1230-1250 oersted at 0%, 780-810 oersted at 5% and ξ210ON, η:
900-97 at 10X and 20% and ξ: 100N
The coercive force in the range of 0 oersteds increases the deposition rate (10 to 20 oersteds).
0 people/viscera) were obtained without being affected.

このように本発明によるとtEU、50度以上の入射角
で斜方入射蒸着金して鉄及び窒化鉄を非磁性基材面に被
着形成する製造方法において、蒸発させた鉄分子に電界
管かけてその5%以上をイオン化するとともに、イオン
銃により窒素分子を前記鉄分子及び鉄イオンに対し5〜
100%の範囲でイオン化し該窒素イオyを前記非磁性
基材面に照射するようにしたから、耐酸化性及び耐磨耗
性の優れた鉄及び窒化鉄から成り、保磁力が600工ル
ステツド以上の磁性薄膜が速い成膜速度で非磁性基材面
に被着形成できると共に、鉄蒸発用電子ビーム用フィラ
メントの寿命が短かくなることがなく、また該フィラメ
ントの近傍で放電が発生しないため故障が発生しない等
の効果を有する。
As described above, according to the present invention, in a manufacturing method in which iron and iron nitride are deposited on a non-magnetic base material surface by obliquely incident evaporation gold at an incident angle of 50 degrees or more, evaporated iron molecules are exposed to an electric field tube. At the same time, an ion gun is used to ionize more than 5% of the iron molecules and iron ions.
Since the nitrogen ions are ionized in a range of 100% and irradiated onto the surface of the non-magnetic base material, it is made of iron and iron nitride with excellent oxidation resistance and wear resistance, and has a coercive force of 600 millimeters. The magnetic thin film described above can be formed on the surface of a non-magnetic substrate at a high deposition rate, and the life of the electron beam filament for iron evaporation will not be shortened, and no discharge will occur near the filament. This has the effect of preventing failures from occurring.

【図面の簡単な説明】[Brief explanation of drawings]

図面は本発明の製造方法を実施するための装置の線図な
示す。 (1)・・・鉄、(2)・・・るつぼ、(3)・・・電
子ビーム放射源、 (4)・・・熱電子放射フィラメント、(5)・・・イ
オン化電極、(6)・・・イオン捕集用電極。 (9)・・・イオン銃。 特許出願人 太陽誌電株式会社 − 外2る
The drawing shows a diagrammatic representation of an apparatus for carrying out the manufacturing method of the invention. (1) Iron, (2) Crucible, (3) Electron beam radiation source, (4) Thermionic emission filament, (5) Ionization electrode, (6) ...Ion collection electrode. (9)...Ion gun. Patent applicant: Taiyo Shiden Co., Ltd.

Claims (1)

【特許請求の範囲】 50度以上の入射角で斜方入射蒸着をして鉄及び脅化鉄
を非磁性基材面に被着形成する式の製造方法において、
蒸発させた鉄分子に電界をかけてその5X以上をイオン
化するとともに、イオン銃によシ窒素分子を前記鉄分子
及び鉄イ。 オンに対し5〜100Xの範囲でイオン化し該窒素イオ
ンを前記非磁性基材面に照射することを特徴とする磁気
記録媒体の製造方法。
[Claims] In a manufacturing method in which iron and threatened iron are deposited on a non-magnetic base material surface by oblique incidence deposition at an incident angle of 50 degrees or more,
An electric field is applied to the evaporated iron molecules to ionize more than 5X of the evaporated iron molecules, and an ion gun is used to ionize the nitrogen molecules and the iron molecules. A method for manufacturing a magnetic recording medium, characterized in that nitrogen ions are ionized in a range of 5 to 100X with respect to nitrogen ions, and the surface of the nonmagnetic base material is irradiated with the nitrogen ions.
JP13442583A 1983-07-25 1983-07-25 Production of magnetic recording medium Granted JPS6028028A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13442583A JPS6028028A (en) 1983-07-25 1983-07-25 Production of magnetic recording medium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13442583A JPS6028028A (en) 1983-07-25 1983-07-25 Production of magnetic recording medium

Publications (2)

Publication Number Publication Date
JPS6028028A true JPS6028028A (en) 1985-02-13
JPH0334621B2 JPH0334621B2 (en) 1991-05-23

Family

ID=15128077

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13442583A Granted JPS6028028A (en) 1983-07-25 1983-07-25 Production of magnetic recording medium

Country Status (1)

Country Link
JP (1) JPS6028028A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160068944A1 (en) * 2014-09-04 2016-03-10 Northwestern University Chemically pure zero-valent iron nanofilms from a low-purity iron source

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160068944A1 (en) * 2014-09-04 2016-03-10 Northwestern University Chemically pure zero-valent iron nanofilms from a low-purity iron source
US9738966B2 (en) * 2014-09-04 2017-08-22 Northwestern University Chemically pure zero-valent iron nanofilms from a low-purity iron source

Also Published As

Publication number Publication date
JPH0334621B2 (en) 1991-05-23

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