JPH0357185B2 - - Google Patents
Info
- Publication number
- JPH0357185B2 JPH0357185B2 JP63127420A JP12742088A JPH0357185B2 JP H0357185 B2 JPH0357185 B2 JP H0357185B2 JP 63127420 A JP63127420 A JP 63127420A JP 12742088 A JP12742088 A JP 12742088A JP H0357185 B2 JPH0357185 B2 JP H0357185B2
- Authority
- JP
- Japan
- Prior art keywords
- sputtering
- vacuum chamber
- plasma source
- substrate
- cathode
- 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.)
- Expired - Lifetime
Links
- 239000000758 substrate Substances 0.000 claims description 35
- 238000004544 sputter deposition Methods 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 238000005192 partition Methods 0.000 claims description 4
- 238000005477 sputtering target Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000010409 thin film Substances 0.000 description 20
- 239000010408 film Substances 0.000 description 17
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 230000004907 flux Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000946 Y alloy Inorganic materials 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は化合物薄膜の形成方法に関し、特に低
温で化合物薄膜を作製する方法に係わるものであ
る。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for forming a compound thin film, and particularly to a method for forming a compound thin film at low temperatures.
［従来の技術］
周知の如く、スパツタリングにより化合物薄膜
を形成する方法として、下記に述べる方法が一般
的である。[Prior Art] As is well known, the method described below is a common method for forming a compound thin film by sputtering.
(1) 酸化物、窒化物等の化合物のターゲツトをス
パツタリングする方法
(2) 反応ガス雰囲気で金属ターゲツトをスパツタ
リングする方法
(3) 金属薄膜を作製し、その後反応ガス雰囲気で
加熱して前記金属薄膜と反応させる方法
［発明が解決しようとする課題］
しかしながら、上記(1)の方法の場合、化合物の
スパツタ率が金属のスパツタ率より低いため、成
膜速度が非常に遅い。また、化合物ターゲツトと
化合物薄膜との組成に差が生じるという問題点を
有する。(1) A method of sputtering a compound target such as an oxide or nitride. (2) A method of sputtering a metal target in a reactive gas atmosphere. (3) A method of producing a metal thin film and then heating it in a reactive gas atmosphere to form the metal thin film. [Problem to be Solved by the Invention] However, in the case of the method (1) above, the sputtering rate of the compound is lower than that of the metal, so the film formation rate is very slow. Another problem is that there is a difference in composition between the compound target and the compound thin film.
上記(2)の方法の場合、金属ターゲツトの表面が
スパツタ中に反応することにより成膜速度が低下
する、基板温度を高くする必要があるなどの問題
点を有する。 In the case of method (2) above, there are problems such as the reaction of the surface of the metal target during sputtering, which reduces the film formation rate, and the need to raise the substrate temperature.
上記(3)の方法の場合、加熱温度が高い、膜厚の
厚い場合には長時間の処理が必要であるなどの問
題点を有する。 In the case of method (3) above, there are problems such as high heating temperature and long processing time required when the film is thick.
本発明は上記事情に鑑みてなされたもので、成
膜速度が大きく、かつ低い基板温度で化合物薄膜
がえられる化合物薄膜の形成方法を提供すること
を目的とする。 The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a method for forming a compound thin film that can be formed at a high film formation rate and at a low substrate temperature.
［課題を解決するための手段］
本発明は、真空槽と、この真空槽内に設けら
れ、スパツタリング用ターゲツトを備えた陰極
と、同真空槽内に設けられた電子サイクロトン共
鳴プラズマ源と、前記陰極とプラズマ源間に設け
られた仕切り板と、前記真空槽内に前記陰極、プ
ラズマ源のいずれにも対向して設けられ、被処理
物を支持する基板ホルダとを具備した装置を用い
て、スパツタリングにより金属薄層を形成した
後、この金属薄層に反応ガスプラズマを照射して
前記金属薄層を反応ガス成分と反応させて化合物
薄層を形成し、この工程を繰返すことを要旨とす
る。[Means for Solving the Problems] The present invention provides a vacuum chamber, a cathode provided in the vacuum chamber and provided with a sputtering target, an electron cycloton resonance plasma source provided in the vacuum chamber, Using an apparatus comprising a partition plate provided between the cathode and the plasma source, and a substrate holder provided in the vacuum chamber facing both the cathode and the plasma source and supporting a processed object. The gist is to form a thin metal layer by sputtering, then irradiate the thin metal layer with reactive gas plasma to react the thin metal layer with the reactive gas component to form a thin compound layer, and repeat this process. do.
［作用］
本発明においては、スパツタリングにより金属
薄層を形成するため成膜速度は化合物をスパツタ
リングするのに比べて非常に大きい。また、この
金属薄層に反応ガスプラズマを照射するため、前
記金属薄膜と反応ガスとの反応が早く、かつ低温
で進行し、短時間で金属薄層が化合物薄層へと変
化し、この繰返しにより低い基板温度、大きな成
膜速度で化合物薄膜を形成することが可能とな
る。[Function] In the present invention, since the metal thin layer is formed by sputtering, the film formation rate is much higher than that when sputtering a compound. In addition, since this metal thin layer is irradiated with reactive gas plasma, the reaction between the metal thin film and the reactive gas proceeds quickly and at a low temperature, and the metal thin layer changes into a compound thin layer in a short time, and this process is repeated. This makes it possible to form a compound thin film at a low substrate temperature and at a high film formation rate.
［実施例］ 以下、本発明の一実施例について説明する。[Example] An embodiment of the present invention will be described below.
まず、本発明に係る薄膜装置について第１図を
参照して説明する。 First, a thin film device according to the present invention will be explained with reference to FIG.
図中の１は、真空槽である。この真空槽１の下
部には、上部にスパツタリング用ターゲツト２を
載置した陰極３が設けられている。また、同真空
槽１の下部で前記陰極３の近くには、CVD時に
用いるECRプラズマ源４が設けられている。こ
のプラズマ源４には、ECRプラズマ源用ガス導
入口５が接続されている。前記陰極３とプラズマ
源４間には、クロスコンタミネーシヨンを避ける
ため仕切り板６が設けられている。前記真空槽１
の上部には、被処理物としての基板７を支持する
回転可能な基板ホルダ８が、前記陰極３、プラズ
マ源４と対向するように配置されている。前記基
板ホルダ８と陰極３、スパツタリング源４間には
シヤツタ９が設けられ、このシヤツタ９の開閉に
より所定の時間のみスパツタリングによる成膜あ
るいはプラズマ照射による反応が起こるようにな
つている。ここで、基板ホルダ８は、スパツタリ
ング時には基板７を前記陰極３に、CVD時には
プラズマ源４に夫々対向させることができるよう
になつている。また、基板ホルダ８の回転を手動
又は自動でスパツタリング及びCVDの動作を連
動させることにより、スパツタリングとECRプ
ラズマCVDとを任意の順序でまた任意回数だけ
連続して行なうことが可能である。前記真空槽１
の側部で前記プラズマ源４側には、ゲートバルブ
１０を備えた排気口１１が設けられている。この
排気口１１をプラズマ源４側に設けるのは、特に
CVD時のプラズマ流がターゲツト２の周囲に達
してターゲツト２を汚染するのを防ぐためであ
る。なお、図中の１２は、スパツタリング用ガス
導入口である。 1 in the figure is a vacuum chamber. A cathode 3 on which a sputtering target 2 is placed is provided at the bottom of the vacuum chamber 1. Further, at the bottom of the vacuum chamber 1 and near the cathode 3, an ECR plasma source 4 used during CVD is provided. This plasma source 4 is connected to an ECR plasma source gas inlet 5 . A partition plate 6 is provided between the cathode 3 and the plasma source 4 to avoid cross contamination. The vacuum chamber 1
A rotatable substrate holder 8 that supports a substrate 7 as an object to be processed is arranged above the cathode 3 and the plasma source 4 so as to face the cathode 3 and the plasma source 4. A shutter 9 is provided between the substrate holder 8, the cathode 3, and the sputtering source 4, and opening and closing of the shutter 9 causes film formation by sputtering or reaction by plasma irradiation to occur only for a predetermined time. Here, the substrate holder 8 is configured so that the substrate 7 can be opposed to the cathode 3 during sputtering and to the plasma source 4 during CVD. Furthermore, by manually or automatically rotating the substrate holder 8 to interlock sputtering and CVD operations, sputtering and ECR plasma CVD can be performed continuously in any order and any number of times. The vacuum chamber 1
An exhaust port 11 equipped with a gate valve 10 is provided on the side of the plasma source 4 . It is especially important to provide this exhaust port 11 on the plasma source 4 side.
This is to prevent the plasma flow during CVD from reaching the surroundings of the target 2 and contaminating the target 2. Note that 12 in the figure is a sputtering gas inlet.
次に、上記した装置を用いて基板上に化合物薄
膜を形成する場合について詳述する。 Next, a case in which a compound thin film is formed on a substrate using the above-described apparatus will be described in detail.
実施例 １
本実施例では、スパツタリング源のターゲツト
として直径4″のFe片を使用し、プラズマ源４の
反応ガスとしてO2ガスを使用し、更に基板とし
て厚さ１mmのガラス板を使用した。Example 1 In this example, a piece of Fe with a diameter of 4'' was used as the target of the sputtering source, O 2 gas was used as the reactive gas of the plasma source 4, and a glass plate with a thickness of 1 mm was used as the substrate.
まず、真空槽１内を予め２×10-7Torrまで排
気した。つづいて、真空槽１内にArガスを導入
して１×10-3Torrとした後、スパツタリングを
行い成膜速度５Å／secで基板７の主面に厚さ15
ÅのFe膜を形成した。次いで、前記基板７がタ
ーゲツト２の真上に位置する状態で基板ホルダ８
を180度回転して基板７をプラズマ源４の真上に
位置するように移動し、この位置でO2プラズマ
を10sec照射した。ここで、プラズマ源４にはO2
ガスを3sccm流し、マイクロ波の出力は300Wであ
る。また、基板の温度は60℃に保持した。この操
作を50回繰返すことにより、厚さ約750Åの化合
物薄膜を得た。 First, the inside of the vacuum chamber 1 was evacuated to 2×10 −7 Torr in advance. Next, after introducing Ar gas into the vacuum chamber 1 to set the pressure to 1×10 -3 Torr, sputtering was performed to form a film on the main surface of the substrate 7 at a film formation rate of 5 Å/sec to a thickness of 15
A Fe film with a thickness of 1.5 nm was formed. Next, with the substrate 7 positioned directly above the target 2, the substrate holder 8 is
was rotated 180 degrees to move the substrate 7 to a position directly above the plasma source 4, and at this position O 2 plasma was irradiated for 10 seconds. Here, the plasma source 4 contains O 2
Gas flows at 3sccm and the microwave output is 300W. Furthermore, the temperature of the substrate was maintained at 60°C. By repeating this operation 50 times, a compound thin film with a thickness of about 750 Å was obtained.
しかして、実施例１によれば、スパツタリング
により基板７の主面にFe膜を形成した後、基板
ホルダ８を回転させて基板７をプラズマ源４の真
上に移動し、この状態でO2ガスプラズマを照射
して化合物薄層を形成し、これらの操作を繰返す
ことにより、所定厚の化合物薄膜を低い基板温度
でしかも大きな成膜速度で作製することができ
る。事実、上記実施例１で得られた化合物薄膜を
Ｘ線回折したところ、得られた膜はγ−Fe2O3で
あることが確認できた。また。VSMの磁気測定
結果、保磁力320（Oe）、飽和磁束密度4300ガウ
ス、残留磁束密度3400ガウス、角型比0.79で、保
磁力、残留磁束密度が高く磁気記録媒体に適した
ものであることが確認できた。また、プラズマ源
として電子サイクロトン共鳴マイクロ波プラズマ
源（ECRプラズマ源）を使用することにより、
より反応性の高いプラズマを得ることができるた
め、化合物形成を効率よく行なうことができる。
なお、前記プラズマ源は動作圧力が低いため、ス
パツタリング源と同一真空槽内で動作させるのに
適している。 According to Example 1, after forming the Fe film on the main surface of the substrate 7 by sputtering, the substrate holder 8 is rotated to move the substrate 7 directly above the plasma source 4, and in this state O 2 By irradiating gas plasma to form a compound thin layer and repeating these operations, a compound thin film of a predetermined thickness can be produced at a low substrate temperature and at a high deposition rate. In fact, when the compound thin film obtained in Example 1 was subjected to X-ray diffraction, it was confirmed that the obtained film was γ-Fe 2 O 3 . Also. The VSM's magnetic measurement results showed a coercive force of 320 (Oe), a saturation magnetic flux density of 4300 Gauss, a residual magnetic flux density of 3400 Gauss, and a squareness ratio of 0.79, indicating that it has a high coercive force and residual magnetic flux density and is suitable for magnetic recording media. It could be confirmed. In addition, by using an electron cycloton resonance microwave plasma source (ECR plasma source) as a plasma source,
Since plasma with higher reactivity can be obtained, compounds can be formed efficiently.
Note that since the plasma source has a low operating pressure, it is suitable for operating in the same vacuum chamber as the sputtering source.
実施例 ２
本実施例では、スパツタリング源のターゲツト
として直径4″のFe片上にBiとＹのチツプを張付
けたものを使用し、プラズマ源４の反応ガスとし
てO2ガスを使用し、更に基板として厚さ0.5mmの
Gd3Ga5O12ガーネツト単結晶板を使用した。Example 2 In this example, a 4" diameter Fe piece with Bi and Y chips attached is used as the target of the sputtering source, O 2 gas is used as the reactive gas of the plasma source 4, and a substrate is used as the substrate. Thickness 0.5mm
A Gd 3 Ga 5 O 12 garnet single crystal plate was used.
まず、真空槽１内を予め２×10-7Torrまで排
気した。つづいて、真空槽１内にArガスを導入
して７×10-3Torrとした後、前記基板７がター
ゲツト２の真上に位置する状態で高周波出力
600Wでスパツタリングを行なつた。同時にプラ
ズマ源４にO2ガスを3sccm流し、マイクロ波出力
300WでO2ガスプラズマを基板７へ照射した。次
いで、この状態で基板ホルダ８を10rpmで回転さ
せ、スパツタリングによるBi−Fe−Ｙ合金薄膜
の形成とO2ガスプラズマ照射を交互に行ない、
成膜時間60minで厚さ2.5μmの化合物薄膜を得た。
なお、基板の温度は200℃に保持した。 First, the inside of the vacuum chamber 1 was evacuated to 2×10 −7 Torr in advance. Next, after introducing Ar gas into the vacuum chamber 1 to set the temperature to 7×10 -3 Torr, high frequency output was performed with the substrate 7 positioned directly above the target 2.
Sputtering was performed at 600W. At the same time, 3 sccm of O 2 gas is flowed into the plasma source 4, and the microwave output is
The substrate 7 was irradiated with O 2 gas plasma at 300W. Next, in this state, the substrate holder 8 is rotated at 10 rpm, and a Bi-Fe-Y alloy thin film is formed by sputtering and O 2 gas plasma irradiation is performed alternately.
A compound thin film with a thickness of 2.5 μm was obtained in a film formation time of 60 min.
Note that the temperature of the substrate was maintained at 200°C.
実施例２で得られた薄膜をＸ線マイクロアナラ
イザーにより組成分析した結果、膜の組成は
Bi2.2Y0.8Fe5.0O12であり、Ｘ線回折の結果ガーネ
ツト単層であることが判明した。 As a result of compositional analysis of the thin film obtained in Example 2 using an X-ray microanalyzer, the composition of the film was found to be
Bi 2.2 Y 0.8 Fe 5.0 O 12 and X-ray diffraction revealed that it was a garnet single layer.
（比較例）
比較のため、上記実施例２と同一のターゲツ
ト、基板を使用し、スパツタリング用のガスとし
てArとO2の混合ガス（Ar：O2＝７：１）を７×
10-3Torrの圧力となるように真空槽内に導入し、
高周波出力600W、基板温度200℃でスパツタリン
グを行なつた。また、基板はスパツタリング源の
真上に静止したままであり、プラズマ源は使用し
なかつた。その結果、成膜時間60minで厚さ
1.5μmの膜が形成された。しかるに、比較例で得
られた薄膜をＸ線マイクロアナライザーにより組
成分析した結果、膜の組成はBi2.0Y1.0Fe5.0O12で
あるが、Ｘ線回折の結果膜は非晶質でありガーネ
ツト相は形成されていないことが判明した。(Comparative Example) For comparison, the same target and substrate as in Example 2 were used, and a mixed gas of Ar and O 2 (Ar:O 2 = 7:1) was used as the sputtering gas at 7×
Introduced into a vacuum chamber to a pressure of 10 -3 Torr,
Sputtering was performed at a high frequency output of 600W and a substrate temperature of 200℃. Also, the substrate remained stationary directly above the sputtering source and no plasma source was used. As a result, the thickness was
A 1.5 μm film was formed. However, as a result of compositional analysis of the thin film obtained in the comparative example with an was found not to have been formed.
［発明の効果］
以上詳述した如く本発明によれば、低い基板温
度でしかも大きな成膜速度で化合物薄膜を形成で
き、もつて基板の種類の選択範囲を広げ、効率も
向上させて工業的にも有利な化合物薄膜の形成方
法を提供できる。[Effects of the Invention] As detailed above, according to the present invention, it is possible to form a compound thin film at a low substrate temperature and at a high film formation rate, thereby expanding the selection range of substrate types, improving efficiency, and improving industrial efficiency. It is also possible to provide a method for forming a compound thin film which is advantageous for the present invention.
第１図は本発明の一実施例に係る成膜装置の説
明図である。
１……真空槽、２……ターゲツト、３……スパ
ツタリング用陰極、４……ECRプラズマ源、５，
１２……ガス導入口、６……仕切り板、７……基
板、８……基板ホルダ、９……シヤツタ、１０…
…ゲートバルブ、１１……排気口。
FIG. 1 is an explanatory diagram of a film forming apparatus according to an embodiment of the present invention. 1... Vacuum chamber, 2... Target, 3... Cathode for sputtering, 4... ECR plasma source, 5,
12... Gas inlet, 6... Partition plate, 7... Substrate, 8... Substrate holder, 9... Shutter, 10...
...gate valve, 11...exhaust port.
Claims (1)
タリング用ターゲツトを備えた陰極と、同真空槽
内に設けられた電子サイクロトン共鳴プラズマ源
と、前記陰極とプラズマ源間に設けられた仕切り
板と、前記真空槽内に前記陰極、プラズマ源のい
ずれにも対向して設けられ、被処理物を支持する
基板ホルダとを具備した装置を用いて、スパツタ
リングにより金属薄層を形成した後、この金属薄
層に反応ガスプラズマを照射して前記金属薄層を
反応ガス成分と反応させて化合物薄層を形成し、
この工程を繰返すことを特徴とする化合物薄膜の
形成方法。1. A vacuum chamber, a cathode provided in the vacuum chamber and provided with a sputtering target, an electron cycloton resonance plasma source provided in the vacuum chamber, and a partition plate provided between the cathode and the plasma source. After forming a thin metal layer by sputtering using an apparatus comprising: a substrate holder which is provided in the vacuum chamber to face both the cathode and the plasma source and supports the object to be processed; irradiating the thin metal layer with a reactive gas plasma to cause the thin metal layer to react with a reactive gas component to form a thin compound layer;
A method for forming a thin compound film characterized by repeating this process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12742088A JPH01298151A (en) | 1988-05-25 | 1988-05-25 | Formation of thin compound film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12742088A JPH01298151A (en) | 1988-05-25 | 1988-05-25 | Formation of thin compound film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01298151A JPH01298151A (en) | 1989-12-01 |
| JPH0357185B2 true JPH0357185B2 (en) | 1991-08-30 |
Family
ID=14959521
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12742088A Granted JPH01298151A (en) | 1988-05-25 | 1988-05-25 | Formation of thin compound film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01298151A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2005087973A1 (en) * | 2004-03-15 | 2008-01-31 | 株式会社アルバック | Film forming apparatus and film forming method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4613015B2 (en) * | 2004-02-10 | 2011-01-12 | 株式会社アルバック | Film forming method and film forming apparatus |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6376867A (en) * | 1986-09-19 | 1988-04-07 | Mitsubishi Kasei Corp | Reactive sputtering device |
-
1988
- 1988-05-25 JP JP12742088A patent/JPH01298151A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6376867A (en) * | 1986-09-19 | 1988-04-07 | Mitsubishi Kasei Corp | Reactive sputtering device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2005087973A1 (en) * | 2004-03-15 | 2008-01-31 | 株式会社アルバック | Film forming apparatus and film forming method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01298151A (en) | 1989-12-01 |
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