JPS63290256A - Manufacture of thin film - Google Patents
Manufacture of thin filmInfo
- Publication number
- JPS63290256A JPS63290256A JP12420787A JP12420787A JPS63290256A JP S63290256 A JPS63290256 A JP S63290256A JP 12420787 A JP12420787 A JP 12420787A JP 12420787 A JP12420787 A JP 12420787A JP S63290256 A JPS63290256 A JP S63290256A
- Authority
- JP
- Japan
- Prior art keywords
- target
- thin film
- partial pressure
- substrate
- gas
- 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 31
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000010408 film Substances 0.000 claims abstract description 29
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000005546 reactive sputtering Methods 0.000 claims abstract description 10
- 239000000376 reactant Substances 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 20
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 2
- 229910001882 dioxygen Inorganic materials 0.000 claims 2
- 239000000758 substrate Substances 0.000 abstract description 21
- 238000004544 sputter deposition Methods 0.000 abstract description 16
- 238000007254 oxidation reaction Methods 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- -1 argon ions Chemical class 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、反応性スパッタリング法を用いた薄１１漠の
製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing a thin film using a reactive sputtering method.
従来の技術
放電ガス中に反応性ガスを混入させる反応性スパッタリ
ング法によシ金属酸化物を形成させたり、さらに反応性
ガスの分圧を制御することにより化合物の組成比を適当
に制御して好ましい物性を引き出す方法が一般に行なわ
れている。Conventional technology A metal oxide is formed by a reactive sputtering method in which a reactive gas is mixed into the discharge gas, and the composition ratio of the compound is appropriately controlled by controlling the partial pressure of the reactive gas. Methods are commonly used to bring out desirable physical properties.
以下第３図を参照しながら上述した方法による薄膜の製
造方法について説明する。第３図は反応性スパッタリン
グ装置の断面図である。図において、１５は内部が排気
可能なチャンバー、１６はチャンバー１５内に配置され
薄膜が形成される基板、１７は基板１６を保持し、かつ
自転ないしは公転させる基板ホルダ、１８は基板１６と
対向して配置された金属ターゲット、１９はターゲット
１８を保持するバッキングプレートである。また２０は
Ａｒガス、２１は０２ガス、２２．２３はガス流量を一
定に保つパルプ、２４は基板１６へのターゲット１８か
らのスパッタ粒子の飛着を制御するシャッタである。The method for manufacturing a thin film using the method described above will be explained below with reference to FIG. FIG. 3 is a cross-sectional view of the reactive sputtering apparatus. In the figure, 15 is a chamber whose inside can be evacuated, 16 is a substrate placed in the chamber 15 and on which a thin film is formed, 17 is a substrate holder that holds the substrate 16 and rotates or revolves around it, and 18 is a substrate that faces the substrate 16. A metal target 19 is a backing plate that holds the target 18. Further, 20 is Ar gas, 21 is 02 gas, 22.23 is pulp that keeps the gas flow rate constant, and 24 is a shutter that controls the adhesion of sputtered particles from target 18 to substrate 16.
次に上記装置の動作を説明する。まず陰極となるターゲ
ット１８及びバッキングプレート１９に高電圧を印加さ
せ、グロー放【Ｅを発生させる。この際、ターゲット１
８表面ではアルゴンイオンあるいは酸素イオンによる表
面原子層のスノくツタリングによる除去とターゲット原
子の酸化反応による表面酸化物層の成長が競合する。こ
のとき相対的に酸化反応がスパッタリングより優勢なと
きには、ターゲット１８表面が酸化物層でおおわれる割
合が大きいが、逆にスパッタリングの方が酸化反応より
優勢なときには、ターゲット１８表面は金属状態のま゛
まである。すなわち、０□ガスの分圧を変化させ酸化速
度を制御することにより、スパッタリングで基板１６上
に形成される薄膜を、はぼ酸化物に近い状態から金属に
近い状態まで変化させることが可能となる。また酸素分
圧を適当に制御することによりＩＴＯ（スズをドープし
た酸化インジウム： Ｉｎｄｉｕｍ Ｔｉｎ ０ｘｉｄ
ｅ）膜の比抵抗及び光学特性を透明電導膜として適した
ものにすることができる。Next, the operation of the above device will be explained. First, a high voltage is applied to the target 18 serving as a cathode and the backing plate 19 to generate glow emission [E]. At this time, target 1
On the 8 surface, the removal of the surface atomic layer by snobbing by argon ions or oxygen ions competes with the growth of the surface oxide layer by the oxidation reaction of the target atoms. At this time, when the oxidation reaction is relatively more dominant than the sputtering, the surface of the target 18 is covered with a large oxide layer, but on the other hand, when the sputtering is more dominant than the oxidation reaction, the surface of the target 18 remains in a metallic state. There are up to ゛. In other words, by changing the partial pressure of the 0□ gas and controlling the oxidation rate, it is possible to change the thin film formed on the substrate 16 by sputtering from a state close to that of an oxide to a state close to a metal. Become. In addition, by appropriately controlling the oxygen partial pressure, ITO (Indium Tin Oxid)
e) The specific resistance and optical properties of the film can be made suitable as a transparent conductive film.
発明が解決しようとする問題点
しかしながら上記のような構成では、Ｔｏのように酸化
しやすい金属をターゲット材料として用いた場合、Ｔｅ
ターゲットが徐々に酸化し、その結果、薄膜の化学組成
および構成が変化する。この現象はターゲットとして焼
結ターゲットを用いた場合顕著である。Problems to be Solved by the Invention However, in the above configuration, when a metal that is easily oxidized like To is used as a target material, Te
The target gradually oxidizes, resulting in a change in the chemical composition and composition of the thin film. This phenomenon is remarkable when a sintered target is used as the target.
一般にＴｅａｘ（０＜ｘ＜２）などの低酸化′＋７０薄
膜は、相変化を利用した光記録膜として用いられるが、
上記の酸化反応によりＸ値が高めに変化することにより
、記録感度が低下し光記録膜として適さなくなる。Generally, low oxidation '+70 thin films such as Teax (0<x<2) are used as optical recording films that utilize phase change.
As the X value changes to a higher value due to the above oxidation reaction, the recording sensitivity decreases and the film becomes unsuitable as an optical recording film.
酸素分圧及び放電電力を一定にし酸化速度及びスパッタ
リング速度を一定にした場合に形成される薄膜の膜厚の
組成分析結果を第４図に示す。これはオージヱ分析を用
いたものである。図において２５はＴｏの組成比、２６
は０の組成比、２７は基板材料のＣの組成比である。こ
の図に示されるように、基板との界面付近でＯ／Ｔ ｅ
比すなわちＩ値が減少するという現象がみられた。これ
は、シャッタ２４を開放して成膜を開始した隙に、ター
ゲット表面の酸化速度とスパッタリング速度のバランス
が一時的にくずれて、酸素が欠乏した膜が初期に形成さ
れ、その後、もとの状態に復帰したためか、あるいは、
基板表面が放電にさらされて形成された薄膜中の酸化物
が分解されたためなどの原因が考えられる。このように
、基板界面から約１００人種度の厚さのところまで所定
の組成からのズレが生じた場合、光記録膜の反射率が１
〜３％程度変化し、これも光記録膜として適さなくなる
。FIG. 4 shows the results of compositional analysis of the thickness of a thin film formed when the oxygen partial pressure and discharge power are kept constant and the oxidation rate and sputtering rate are kept constant. This uses audio analysis. In the figure, 25 is the composition ratio of To, 26
is the composition ratio of 0, and 27 is the composition ratio of C of the substrate material. As shown in this figure, O/T e near the interface with the substrate
A phenomenon was observed in which the ratio, that is, the I value decreased. This is because when the shutter 24 is opened and film formation begins, the balance between the oxidation rate of the target surface and the sputtering rate is temporarily lost, and an oxygen-deficient film is initially formed, and then the original film is formed. Perhaps because the condition has returned to normal, or
Possible causes include decomposition of oxides in the thin film formed when the substrate surface is exposed to electric discharge. In this way, if a deviation from the predetermined composition occurs up to a thickness of about 100 degrees from the substrate interface, the reflectance of the optical recording film will decrease by 1.
It changes by about 3%, which also makes it unsuitable as an optical recording film.
問題点を解決するための手段
上記問題点を解決するために本発明の薄膜製造方法は、
反応性ガスの分圧を上げて（ブリスパッタ）を行い、タ
ーゲット上に過剰に表面反応層をを形成させてから成膜
を開始するものである。Means for Solving the Problems In order to solve the above problems, the thin film manufacturing method of the present invention includes:
Film formation is started after increasing the partial pressure of the reactive gas (bliss sputtering) to form an excessive surface reaction layer on the target.
作 用
上記の方法により、反応ガスの分圧を上げてあらかじめ
ブリスパッタを行ない、ターゲット表面に過剰な反応物
を形成して成膜中の薄膜組成の変動を補償し形成薄膜の
組成を二定にする。Effect: By the above method, the partial pressure of the reactant gas is increased and bliss sputtering is performed in advance to form excess reactants on the target surface to compensate for fluctuations in the thin film composition during film formation and to keep the composition of the formed thin film constant. do.
実施例
以下、本発明の一実施例について図面を参照して説明す
る。第１図は反応性スパッタリング装置の断面図である
。１は内部が排気可能なチャンバー、２はチャンバー１
内に配置され薄膜が形成される基板、３は基板２を保持
しかつ自転ないしは公転させるホルダ、４は基板２と対
向して配置された金属ターゲット、５はターゲット４を
保持するバンキングプレート、６はバッキングプレート
６を冷却する冷却水である。また７はＡｒガス、８は０
２ガス、９，１０はガス流量を制御するコントロールパ
ルプ、１１は基板２へのターゲット４からのスパッタ粒
子の飛着を制御するシャッタである。EXAMPLE Hereinafter, an example of the present invention will be described with reference to the drawings. FIG. 1 is a sectional view of a reactive sputtering apparatus. 1 is a chamber whose inside can be evacuated, 2 is a chamber 1
3 is a holder that holds the substrate 2 and rotates or revolves around it; 4 is a metal target that is placed facing the substrate 2; 5 is a banking plate that holds the target 4; 6; is cooling water that cools the backing plate 6. Also, 7 is Ar gas, 8 is 0
2 gases, 9 and 10 are control pulps that control gas flow rates, and 11 is a shutter that controls the flying of sputtered particles from the target 4 onto the substrate 2.
次に動作を説明する。まず、陰極となるターゲット４及
びバッキングプレート６に高電圧を印加し、グロー放電
を発生させる。このときターゲット４表面ではアルゴン
イオンあるいは酸素イオンによる表面原子層のスパッタ
リングによる除去とターゲット原子の酸化反応による狭
面酸化物層の成長が同時に起こる。この際、スパッタリ
ング速度及び酸化速度を変えることによシスノ・：ノタ
リングで形成される薄膜をほぼ酸化物に近い状態から金
属に近い状態まで変化させることが可能となる。Next, the operation will be explained. First, a high voltage is applied to the target 4 serving as a cathode and the backing plate 6 to generate glow discharge. At this time, on the surface of the target 4, the removal of the surface atomic layer by sputtering using argon ions or oxygen ions and the growth of a narrow-sided oxide layer due to the oxidation reaction of the target atoms occur simultaneously. At this time, by changing the sputtering rate and the oxidation rate, it is possible to change the thin film formed by cysno:notaring from a state close to an oxide to a state close to a metal.
スパッタリング速度を制御する手段として投入電力制御
がまた、酸化速度を変える手段としでへガス分圧すなわ
ちＱ２ガス流量制御が用いられる。Input power control is used as a means for controlling the sputtering rate, and gas partial pressure control, that is, Q2 gas flow rate control, is used as a means for changing the oxidation rate.
これらを適当に制御することにより形成薄膜の組成及び
特性を変えることができる。ターゲット４材料としてＴ
ｅを用いた場合、形成薄膜としてＴｏｏ （０＜！＜
２）薄膜が形成される。この薄膜を相変化型の光記録膜
として用いる場合、Ｔｅと酸素の比がおおよそ１：１の
ときが最も感度が高くかつ安定であることが報告されて
いる（第２８回応用物理学関係連合溝演会子稿集３１ｐ
−Ｒ−７〜１２（１９８１））。したがって投入電力及
び０２ガス流量を適当に制御してＴｏｏ工膜のＸ値を１
にする。By appropriately controlling these, the composition and properties of the formed thin film can be changed. T as target 4 material
When using e, Too (0<!<
2) A thin film is formed. When using this thin film as a phase-change optical recording film, it has been reported that the highest sensitivity and stability are achieved when the ratio of Te and oxygen is approximately 1:1 (28th Union of Applied Physics Mizoenkai manuscript collection 31 pages
-R-7 to 12 (1981)). Therefore, by appropriately controlling the input power and the 02 gas flow rate, the X value of the Too film can be reduced to 1.
Make it.
このときの投入電力は４００Ｗ、０２ガス流量は２０Ｓ
ＣＣＭだった。The input power at this time was 400W, and the 02 gas flow rate was 20S.
It was CCM.
投入電力を一定にしたま−まｏ２ガス流量を２６ＳＣＣ
Ｍにしてブリスパッタを行うとターゲット４表面上に過
剰な酸化物層が形成される。この状態でシャッタ１１を
開放して成膜を開始すると、シャッタ移動にともなうタ
ーゲット表面の放電プラズマ状態の変化や、基板へのタ
ーゲット４からの２次電子等の流入により１女化物の分
解が起こり、脱離した酸素はチャンバ１から排気される
。。したがってターゲット表面の過剰な酸化物層は急速
に分解され、成膜開始直後から形成されるＴｅＯｘ膜は
Ｘ値が１と理想的な膜となる。その後、ｏ２ガス流量を
２０ＳＣＣＭに戻してスパッタを続けると、ターゲット
４表面の酸化物層の分解とターゲット自体の酸化が平衡
するため、成膜の全期間を通して一定した組成の薄膜が
安定して得られる。While the input power is constant, the O2 gas flow rate is 26SCC.
When bliss sputtering is performed with M, an excessive oxide layer is formed on the surface of the target 4. When the shutter 11 is opened to start film formation in this state, the decomposition of the 1-female compound occurs due to changes in the discharge plasma state on the target surface as the shutter moves and secondary electrons flowing into the substrate from the target 4. , the desorbed oxygen is exhausted from chamber 1. . Therefore, the excessive oxide layer on the target surface is rapidly decomposed, and the TeOx film formed immediately after the start of film formation becomes an ideal film with an X value of 1. After that, when the O2 gas flow rate is returned to 20SCCM and sputtering is continued, the decomposition of the oxide layer on the surface of the target 4 and the oxidation of the target itself are balanced, so a thin film with a constant composition can be stably obtained throughout the entire film formation period. It will be done.
このときの膜厚方向の組成分析結果を第２図に示す。こ
れはオージェ分析をしたものである。横軸は薄膜の深さ
方向（人）で、縦軸は組成比である。１２はＴｏの組成
比、１３は０の組成比、１４は基板材料のＣの組成比で
ある。The compositional analysis results in the film thickness direction at this time are shown in FIG. This is an Auger analysis. The horizontal axis is the depth direction (person) of the thin film, and the vertical axis is the composition ratio. 12 is the composition ratio of To, 13 is the composition ratio of 0, and 14 is the composition ratio of C of the substrate material.
第２図から明らかなように本芙施例によれば、従来みら
れた基板との界面付近での薄膜の酸素欠乏はみられず、
薄膜の厚さ方向の全域でＴｏｏ工のＸ値が約１と光記録
膜として適した膜の製造が可能となった。As is clear from FIG. 2, according to this example, oxygen depletion in the thin film near the interface with the substrate, which was observed in the past, was not observed.
It has become possible to manufacture a film suitable as an optical recording film with a Too's X value of about 1 over the entire thickness direction of the thin film.
発明の効果
以上のように本発明の薄膜の製造方法は、反応性ガスの
分圧を上げてブリスパッタを行ない、ターゲット上に過
剰に表面反応物層を形成させてから成膜を開始するもの
であり、本発明の方法により成膜中の薄膜組成の変動を
補償して形成薄膜の組成を一定にすることができる。ま
たこのことにより反応性スパッタ法において安定した組
成および特性の薄膜の製造が可能となり、品質の向上お
よび生産性の向上に大いに役立つものである。Effects of the Invention As described above, the thin film manufacturing method of the present invention involves increasing the partial pressure of a reactive gas and performing bliss sputtering to form an excessive surface reactant layer on the target before starting film formation. According to the method of the present invention, variations in the composition of the thin film during film formation can be compensated for and the composition of the formed thin film can be made constant. Furthermore, this makes it possible to produce a thin film with stable composition and properties by reactive sputtering, which is of great help in improving quality and productivity.
第１図は本発明の一実施例に用いたスパッタリング装置
の断面図、第２図は本発明の方法を用いて形成した薄膜
の厚さ方向の組成分析結果を示したグラフ、第３図は従
来の方法に用いたスパッタリング装置の断面図、第４図
は従来の方法を用いて形成した薄膜の厚さ方向の組成分
析結果を示したグラフである。
２・・・・・・基板、４・・・・・・ターゲット、９．
１０・・・・・・コントロールパルフ、１１・・・・・
・シャッタ、１２・・・・・・Ｔｏの組成比、１３・・
・・・・０の組成比。
代理人の氏名 弁理士 中 尾 敏 男 ほか１名第
２ 図
膜表面から９深さくｌノ
第４図
膜表面Ｄ１うの深さ ＜Ａ）FIG. 1 is a cross-sectional view of a sputtering apparatus used in an embodiment of the present invention, FIG. 2 is a graph showing the composition analysis results in the thickness direction of a thin film formed using the method of the present invention, and FIG. FIG. 4, which is a sectional view of a sputtering apparatus used in the conventional method, is a graph showing the compositional analysis results in the thickness direction of a thin film formed using the conventional method. 2...Substrate, 4...Target, 9.
10...Control palf, 11...
・Shutter, 12... Composition ratio of To, 13...
...0 composition ratio. Name of agent: Patent attorney Toshio Nakao and 1 other person
2. Depth of 9 depths from the membrane surface in Figure 4. Depth of membrane surface D1 <A)
Claims (2)
ゲット上に過剰に表面反応物層を形成させ、その後、反
応性スパッタリング法による成膜を開始する薄膜の製造
方法。(1) A method for producing a thin film in which a preliminary discharge is performed by increasing the partial pressure of a reactive gas to form an excessive surface reactant layer on a target, and then film formation by a reactive sputtering method is started.
ト上に過剰に表面酸化物層を形成させ、しかる後、反応
性スパッタリング法による成膜を開始し、その後、酸素
ガス分圧を下げて再び反応性スパッタリング法で薄膜を
形成する特許請求の範囲第１項記載の薄膜の製造方法。(2) Increase the partial pressure of oxygen gas by 20% or more to form an excessive surface oxide layer on the target, then start film formation by reactive sputtering, and then reduce the partial pressure of oxygen gas. 2. The method of manufacturing a thin film according to claim 1, wherein the thin film is formed again by a reactive sputtering method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12420787A JPH0768615B2 (en) | 1987-05-21 | 1987-05-21 | Thin film manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12420787A JPH0768615B2 (en) | 1987-05-21 | 1987-05-21 | Thin film manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63290256A true JPS63290256A (en) | 1988-11-28 |
| JPH0768615B2 JPH0768615B2 (en) | 1995-07-26 |
Family
ID=14879641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12420787A Expired - Lifetime JPH0768615B2 (en) | 1987-05-21 | 1987-05-21 | Thin film manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0768615B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04160144A (en) * | 1990-10-24 | 1992-06-03 | Nec Corp | Production of dielectric film |
| US7049190B2 (en) | 2002-03-15 | 2006-05-23 | Sanyo Electric Co., Ltd. | Method for forming ZnO film, method for forming ZnO semiconductor layer, method for fabricating semiconductor device, and semiconductor device |
| JP2019138971A (en) * | 2018-02-07 | 2019-08-22 | 凸版印刷株式会社 | Reflective photomask blank and reflective photomask |
-
1987
- 1987-05-21 JP JP12420787A patent/JPH0768615B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04160144A (en) * | 1990-10-24 | 1992-06-03 | Nec Corp | Production of dielectric film |
| JP2581300B2 (en) * | 1990-10-24 | 1997-02-12 | 日本電気株式会社 | Manufacturing method of dielectric film |
| US7049190B2 (en) | 2002-03-15 | 2006-05-23 | Sanyo Electric Co., Ltd. | Method for forming ZnO film, method for forming ZnO semiconductor layer, method for fabricating semiconductor device, and semiconductor device |
| JP2019138971A (en) * | 2018-02-07 | 2019-08-22 | 凸版印刷株式会社 | Reflective photomask blank and reflective photomask |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0768615B2 (en) | 1995-07-26 |
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