JPS6365611A - Formation of ferromagnetic thin film - Google Patents
Formation of ferromagnetic thin filmInfo
- Publication number
- JPS6365611A JPS6365611A JP21016086A JP21016086A JPS6365611A JP S6365611 A JPS6365611 A JP S6365611A JP 21016086 A JP21016086 A JP 21016086A JP 21016086 A JP21016086 A JP 21016086A JP S6365611 A JPS6365611 A JP S6365611A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- substrate
- temperature
- heater
- target
- 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
- 239000010409 thin film Substances 0.000 title claims abstract description 34
- 230000005294 ferromagnetic effect Effects 0.000 title claims description 7
- 230000015572 biosynthetic process Effects 0.000 title 1
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000000956 alloy Substances 0.000 claims abstract description 3
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- 229910052779 Neodymium Inorganic materials 0.000 claims 1
- 229910052777 Praseodymium Inorganic materials 0.000 claims 1
- 229910052772 Samarium Inorganic materials 0.000 claims 1
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- 238000004544 sputter deposition Methods 0.000 abstract description 9
- 230000005291 magnetic effect Effects 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Thin Magnetic Films (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は磁気記録媒体や高性能小型モータなどに用い
られる最大エネルギ積（ＢＨ） ｍａｘの大きい強磁性
薄膜の形成方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for forming a ferromagnetic thin film having a large maximum energy product (BH) max used in magnetic recording media, high-performance small motors, and the like.
（従来の技術）
このような強磁性薄膜の形成方法として特開昭４９−８
６８９５が提案されている。これは膜を付着する下地の
基板温度を２０℃に冷却した状態で高速スパッタリング
を行い、数１０μｍの膜を形成した後アニール処理を行
う方法である。これによって保磁力ｉＨｃが３５ ｋＯ
ｅ、最大エネルギ積（ＢＨ） ｍａｘが１０ ＭＧＯｅ
の特性を得ている。(Prior art) As a method for forming such a ferromagnetic thin film, Japanese Patent Application Laid-Open No. 49-8
6895 has been proposed. This is a method in which high-speed sputtering is performed with the substrate temperature on which the film is attached cooled to 20° C., and after a film of several tens of micrometers is formed, an annealing treatment is performed. This results in a coercive force iHc of 35 kO.
e, maximum energy product (BH) max is 10 MGOe
It has obtained the characteristics of
また、 ａ Ｈ，Ａｌｙ等はＳｍＣｏ ５の薄膜を形成
して面内方向で２０ ＭＧＯｅの（ＢＨ） ｍａｘを得
ているが、膜厚方向の特性は非常に小さいものである（
Ｊ、ＡｐｐＬＰｈｙｓ、、 ５７ （８１，１５Ｍａｒ
ｃｈ １９８５Ｐ、２１４９）。In addition, aH, Aly, etc. have obtained a (BH) max of 20 MGOe in the in-plane direction by forming a thin film of SmCo 5, but the characteristics in the film thickness direction are very small (
J, AppLPhys, 57 (81,15 Mar
ch 1985P, 2149).
（発明が解決しようとする問題点）
磁気を利用した装置を高性能化または小型化する場合に
は膜厚方向の最大エネルギ積（ＢＨ）ｍａｘの大きいこ
と、たとえば１０ ＭＧＯｅ以上のものが必要である。(Problem to be solved by the invention) In order to improve the performance or downsize a device using magnetism, it is necessary to have a large maximum energy product (BH) max in the film thickness direction, for example, 10 MGOe or more. be.
しかし、従来の薄膜形成方法によってはこのような値が
得られていないのが現状である。また、基板の温度を２
０℃に保持してスパッタリングを行うには冷却装置が必
要となるため基板の形状が制限される欠点がある。However, the current situation is that such values cannot be obtained using conventional thin film forming methods. Also, the temperature of the board is 2
Since a cooling device is required to perform sputtering while maintaining the temperature at 0° C., there is a drawback that the shape of the substrate is limited.
（本発明の目的）
この発明は上記の問題点を解決した最大工ネルギ積（Ｂ
Ｈ） ｍａｘの高い薄膜の形成方法を提供するものであ
る。(Objective of the present invention) This invention solves the above-mentioned problems and solves the problems described above.
H) A method for forming a thin film with high max is provided.
（問題点を解決するための手段）
このため１本発明は、希土類ＲとＣｏとの合金ＦｔｔＲ
をスパッタリングによって形成する際に基板温度を１５
０℃〜３５０℃に保持して薄膜を形成した後、真空中も
しくは非酸化性雰囲気中にて６ｓｏｇｏｏ℃でアニール
を行うようにしである。(Means for solving the problem) For this reason, the present invention provides an alloy FttR of rare earth R and Co.
When forming by sputtering, the substrate temperature was set to 15
After forming a thin film while maintaining the temperature at 0° C. to 350° C., annealing is performed at 60° C. in vacuum or in a non-oxidizing atmosphere.
（作用）
上記のように基板温度を１５０℃〜３５０℃にすること
によって形成された薄膜の構造は非晶質もしくは微細結
晶となり、この後の６５０’Ｃ〜８００℃のアニールに
よって十分な結晶化が計れるため、高エネルギ積の磁気
特性を有する薄膜が得られる。(Function) The structure of the thin film formed by raising the substrate temperature to 150°C to 350°C as described above becomes amorphous or microcrystalline, and is sufficiently crystallized by subsequent annealing at 650°C to 800°C. can be measured, resulting in a thin film having magnetic properties with a high energy product.
（実施例） 以下この発明を実施例によって詳細に説明する。(Example) The present invention will be explained in detail below with reference to Examples.
第１実施例
第１図はこの発明の薄膜形成に用いたＤＣ２極マグネト
ロンスパッタリング装置の概略図である。真空容器１の
中には薄膜中のＳｍの原子比が２０９６になるようにＳ
ｍ粉末とＣｏ粉末とを混合した後真空中で焼結して得た
ターゲット２、ターゲットから３５ｍｍの距離に対向さ
せた基板３．基板の取付は台４．シャッタ５．基板背後
に設置した基板加熱用ヒータ６が配置されている。まず
、真空容器内をＩ Ｘ １０−５ Ｔｏｒｒ以下に排気
した後、ヒータ６に交流電流を通じて、基板、基板取付
は台及びターゲットなどを４００℃以上に約２時間加熱
してベーキングを行い、この後１００℃以下になるまで
冷却した。First Embodiment FIG. 1 is a schematic diagram of a DC bipolar magnetron sputtering apparatus used for forming a thin film according to the present invention. Inside the vacuum container 1, S is added so that the atomic ratio of Sm in the thin film is 2096.
A target 2 obtained by mixing M powder and Co powder and sintering in vacuum, and a substrate 3 facing the target at a distance of 35 mm. Mount the board on stand 4. Shutter 5. A heater 6 for heating the substrate is placed behind the substrate. First, after evacuating the inside of the vacuum chamber to below IX 10-5 Torr, an alternating current is passed through the heater 6 to heat the substrate, the base for mounting the substrate, the target, etc. to 400°C or higher for about 2 hours to perform baking. It was then cooled to below 100°C.
つぎに、 Ａｒガス導入パルプ８を開いてＡｒガスを導
入し、圧力を０．０２〜０．０４Ｔｏｒｒに調整した後
、シャッタ５を閉じた状態でターゲット２に３５０Ｖ〜
３５０ｖの直流電圧を印加して約２０ｍＡ／ｄのターゲ
ット電流を約２０分間通じて予備スパッタリングを行い
、ターゲット表面の酸化物を除去した。この後バイアス
電源９を調整して負の直流電圧６０Ｖを印加してシャッ
タを開き、２０〜２５ ｍＡ／ ｃｄのターゲット電流
を１時間通じてスパッタリングを行い薄膜を形成した。Next, the Ar gas introducing pulp 8 is opened to introduce Ar gas, and after adjusting the pressure to 0.02 to 0.04 Torr, a voltage of 350 V to 350 V is applied to the target 2 with the shutter 5 closed.
Preliminary sputtering was performed by applying a DC voltage of 350 V and passing a target current of about 20 mA/d for about 20 minutes to remove oxides on the target surface. Thereafter, the bias power supply 9 was adjusted, a negative DC voltage of 60 V was applied, the shutter was opened, and a target current of 20 to 25 mA/cd was applied to perform sputtering for 1 hour to form a thin film.
この場合の基板温度はヒータ６にわずかに電流を通じて
予熱し３５０℃とした。つぎにシャッタを閉じて真空容
器内をＩ Ｘ １０−５Ｔｏｒｒ以下の圧力に排気し、
ヒータ６に電流を通じて基板を７００℃に加熱し、この
温度で６０分間保持した後、室温まで冷却した。このよ
うにして形成した薄膜の膜厚方向に超電導コイルを用い
て８０ｋＯｅの外部磁界を印加し。In this case, the substrate temperature was set to 350° C. by passing a slight current through the heater 6 to preheat it. Next, close the shutter and evacuate the inside of the vacuum container to a pressure of I x 10-5 Torr or less,
The substrate was heated to 700° C. by passing an electric current through the heater 6, held at this temperature for 60 minutes, and then cooled to room temperature. An external magnetic field of 80 kOe was applied in the thickness direction of the thin film thus formed using a superconducting coil.
磁気特性を測定した結果、 １４ＭＧＯｅの最大エネ
ルギ積（ＢＨ） ｍａｘの値が得られた。この薄膜のＳ
ｍ濃度を調べるため組成分析を行ったところＳｍの原子
比は１８％で残りＣｏとなっておりほぼＳｍＣｏ５系の
組成となっていた。As a result of measuring the magnetic properties, a maximum energy product (BH) max value of 14MGOe was obtained. The S of this thin film
A compositional analysis was performed to check the m concentration, and the atomic ratio of Sm was 18%, with the remainder being Co, making the composition almost SmCo5-based.
さらに、基板温度を１００〜４００℃の範囲で薄膜を作
成した。基板温度が１００〜２５０℃の範囲ではヒータ
による予熱を行うことなしに、ターゲット電流の大きさ
で調整した。この後６００〜８５０℃の種々の温度でア
ニールを行った後、前記と同様にして（ＢＨ） ｍａｘ
を求め、基板温度とアニール温度についてプロットした
ところ第２図に示す結果が得られた。図中の数字は（Ｂ
Ｈ） ｍａｘの値であり、線で囲んだ範囲Ａは（ＢＨ）
ｍａｘが１０ ＭＧＯｅを越える値が得られた条件で
ある。この範囲内で形成された薄膜は結晶化が最適にな
ったものと考えられる。 なお、最大エネルギ積（ＢＨ
） ｍａ：ｃに対する組成の影響を調べるためにＳｍ粉
末とＣｏ粉末の混合割合を種々変えた焼結ターゲットを
作製し、基板温度を２５０℃とし、他の条件は前記と同
様にしてスパッタリングを行って薄膜を形成した。この
後真空中にて７００℃１時間のアニールを施した。Ｓｍ
の原子比が２５％及び３５９６の薄膜の最大エネルギ積
は１２〜１３ ＭＧＯｅであったが、 Ｓｍの原子比が
１３％及び４０９６の薄膜では１０ＭＧＯｅ以下と低い
値であった。Furthermore, thin films were created with the substrate temperature in the range of 100 to 400°C. When the substrate temperature was in the range of 100 to 250° C., the target current was adjusted without preheating with a heater. After this, annealing was performed at various temperatures from 600 to 850°C, and then (BH) max
When the substrate temperature and annealing temperature were plotted, the results shown in FIG. 2 were obtained. The numbers in the figure are (B
H) is the value of max, and the range A surrounded by the line is (BH)
These are the conditions under which a value of max exceeding 10 MGOe was obtained. It is considered that the thin film formed within this range has optimal crystallization. In addition, the maximum energy product (BH
) In order to investigate the influence of composition on ma:c, sintered targets were prepared with various mixing ratios of Sm powder and Co powder, and sputtering was performed at a substrate temperature of 250 °C and other conditions as above. A thin film was formed. Thereafter, annealing was performed at 700° C. for 1 hour in a vacuum. Sm
The maximum energy product of a thin film with an Sm atomic ratio of 25% and 3596 was 12 to 13 MGOe, but a thin film with an Sm atomic ratio of 13% and 4096 had a low value of 10 MGOe or less.
また、 Ｓｍ濃度が１８原子％の膜が得られる前記ター
ゲットに５０〜５００Ｗの高周波電圧を印加して形成し
た後７＆で１時間アニールした薄膜についても１２ＭＧ
Ｏｅの最大エネルギ積が得られた。さらに、薄膜を形成
した後。Furthermore, a thin film formed by applying a high frequency voltage of 50 to 500 W to the target to obtain a film with an Sm concentration of 18 at %, and then annealed for 1 hour at 7&msp; was also 12 MG.
A maximum energy product of Oe was obtained. Furthermore, after forming a thin film.
アニールを施す際に膜が酸化されないＨ２ガスやＡｒガ
ス雰囲気中で処理した場合も１０ ＭＧＯｅ以上の最大
エネルギ積の値が得られた。Even when annealing was performed in an H2 gas or Ar gas atmosphere in which the film is not oxidized, a maximum energy product value of 10 MGOe or more was obtained.
第２実施例
薄膜中のＰｒの原子比が２０９６になるようにＰｒ粉末
とＣｏ粉末とを混合して真空中で焼結しターゲットを作
製し、第１実施例と同様に直流２極スパツタリングで薄
膜を形成した。この後高真空中にて７誹もで１時間のア
ニールを施した。磁気測定を行い最大エネルギ積を求め
たところ基板温度１５０℃、２５０℃、３５０℃で１２
ＭＧＯｅの値を得た。Second Example A target was prepared by mixing Pr powder and Co powder so that the atomic ratio of Pr in the thin film was 2096 and sintering in vacuum, and using DC bipolar sputtering as in the first example. A thin film was formed. Thereafter, annealing was performed in a high vacuum for 1 hour at 7 increments. When we performed magnetic measurements and found the maximum energy product, it was 12 at substrate temperatures of 150°C, 250°C, and 350°C.
The value of MGOe was obtained.
（発明の効果）
以上説明したようにこの発明によればスパッタリング時
の基板の温度を冷却または高温に加熱する必要がないた
め、基板の形状に制限なく最大エネルギ積（ＢＨ） ｍ
ａｘΦ大きい薄膜が得られる。(Effects of the Invention) As explained above, according to the present invention, there is no need to cool down or heat the substrate to a high temperature during sputtering, and therefore the maximum energy product (BH) m is not limited to the shape of the substrate.
A thin film with a large axΦ can be obtained.
このため、磁気を別層した高性能小型モータ及び磁気記
録媒体への適用が可能な強磁性薄膜を得ることができる
。Therefore, it is possible to obtain a ferromagnetic thin film that can be applied to high-performance small motors and magnetic recording media with separate magnetic layers.
第１図はこの発明の強磁性薄膜の形成に用いた装置の概
略図、第２図は最大エネルギ積（ＢＨ）ｍａＸと薄膜形
成条件との関係を示した図である。
２はターゲット、３は基板、６は携沖１察ヒータである
。
第１図
５、シャッタ −０．ヒータ電源箱 ２ 回
基板温度（°Ｃ）FIG. 1 is a schematic diagram of the apparatus used for forming the ferromagnetic thin film of the present invention, and FIG. 2 is a diagram showing the relationship between the maximum energy product (BH) maX and the thin film forming conditions. 2 is a target, 3 is a board, and 6 is a portable heater. Figure 1 5, shutter -0. Heater power supply box 2 times Board temperature (°C)
Claims (1)
なる希土類金属ＲとＣｏからなる合金薄膜を、基板温度
１５０℃〜３５０℃にてスパッタリングを行い、Ｒの原
子比が１５〜３５％を占めるように形成し、真空中もし
くは非酸化性雰囲気中において６５０℃〜８００℃でア
ニールすることを特徴とする強磁性薄膜の形成方法。A thin alloy film made of a rare earth metal R made of at least one of Sm, Pr, Ce, Nd, and Y and Co is sputtered at a substrate temperature of 150°C to 350°C, and the atomic ratio of R is 15 to 35%. A method for forming a ferromagnetic thin film, which comprises forming the ferromagnetic thin film as described above and annealing it at 650°C to 800°C in vacuum or in a non-oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21016086A JPS6365611A (en) | 1986-09-05 | 1986-09-05 | Formation of ferromagnetic thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21016086A JPS6365611A (en) | 1986-09-05 | 1986-09-05 | Formation of ferromagnetic thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6365611A true JPS6365611A (en) | 1988-03-24 |
| JPH0571165B2 JPH0571165B2 (en) | 1993-10-06 |
Family
ID=16584756
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21016086A Granted JPS6365611A (en) | 1986-09-05 | 1986-09-05 | Formation of ferromagnetic thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6365611A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5062938A (en) * | 1990-01-16 | 1991-11-05 | International Business Machines Corporation | High coercivity low noise cobalt alloy magnetic recording medium and its manufacturing process |
| US7905991B2 (en) * | 2004-11-12 | 2011-03-15 | Oerlikon Trading Ag, Trubbach | Vacuum treatment system |
-
1986
- 1986-09-05 JP JP21016086A patent/JPS6365611A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5062938A (en) * | 1990-01-16 | 1991-11-05 | International Business Machines Corporation | High coercivity low noise cobalt alloy magnetic recording medium and its manufacturing process |
| US7905991B2 (en) * | 2004-11-12 | 2011-03-15 | Oerlikon Trading Ag, Trubbach | Vacuum treatment system |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0571165B2 (en) | 1993-10-06 |
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