JP3107638B2 - Measuring method of metal thin film quality - Google Patents
Measuring method of metal thin film qualityInfo
- Publication number
- JP3107638B2 JP3107638B2 JP04070633A JP7063392A JP3107638B2 JP 3107638 B2 JP3107638 B2 JP 3107638B2 JP 04070633 A JP04070633 A JP 04070633A JP 7063392 A JP7063392 A JP 7063392A JP 3107638 B2 JP3107638 B2 JP 3107638B2
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- Prior art keywords
- thin film
- metal thin
- quality
- measuring
- film
- Prior art date
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は金属薄膜の膜質の測定方
法に関し、特に半導体装置において配線用金属薄膜とし
て用いられるＡｌまたはＡｌ合金薄膜の膜質の測定方法
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the quality of a metal thin film, and more particularly to a method for measuring the quality of an Al or Al alloy thin film used as a metal thin film for wiring in a semiconductor device.
【０００２】[0002]
【従来の技術】金属薄膜の形成方法には、スパッタリン
グ、加熱蒸着、イオンプレ−ティング、及びメッキなど
である。それらいずれの方法においても、良質な膜質を
得るためには、金属薄膜中の不純物量を減らすことが重
要である。2. Description of the Related Art Methods for forming a metal thin film include sputtering, heat evaporation, ion plating, and plating. In any of these methods, it is important to reduce the amount of impurities in the metal thin film in order to obtain good film quality.
【０００３】そのため従来から採用されている方法は、
（１）金属薄膜の原料純度を向上させる、（２）反応室
内の雰囲気を一定の水準に維持して汚染を減らす、こと
である。具体的には、次のように行う。（１）は、材料
の分析をすることにより使用材料の品質を一定に保つ方
法である。（２）は、反応室内の残留不純物成分の分析
をすること、又は薄膜形成後の薄膜の硬度や比抵抗など
の物性値から、反応室内の雰囲気を調べ方法である。[0003] Therefore, the method conventionally used is:
(1) to improve the purity of the raw material of the metal thin film; and (2) to reduce contamination by maintaining the atmosphere in the reaction chamber at a constant level. Specifically, this is performed as follows. (1) is a method of keeping the quality of the used material constant by analyzing the material. The method (2) is a method of analyzing a residual impurity component in the reaction chamber or examining the atmosphere in the reaction chamber from physical properties such as hardness and specific resistance of the thin film after forming the thin film.
【０００４】ところで、原料の純度に関しては、従来よ
りかなり精度よく管理されているため殆ど問題がない。
これに対し、薄膜形成中、不純物の混入を察知して抑制
することは難しい。特に半導体装置を製造をする際に
は、不純物の混入量を測定するのは非常に困難である。[0004] By the way, there is almost no problem with regard to the purity of the raw material since it is controlled with considerably higher accuracy than in the past.
On the other hand, it is difficult to detect and suppress the entry of impurities during the formation of the thin film. In particular, when manufacturing a semiconductor device, it is very difficult to measure the amount of impurities mixed.
【０００５】しかしながら、半導体装置において配線用
金属として多く用いられるＡｌは、スパッタ室内の不純
物ガスの影響を受けやすくＨ2 Ｏ，Ｎ2 ，Ｏ2 ，ＣＯ，
ＣＯ2 等により膜質は著しく変わってくる。そのため、
スパッタ室内の不純物ガス量に関心を示すことは重要と
なる。However, Al, which is often used as a wiring metal in a semiconductor device, is susceptible to impurity gases in a sputtering chamber, and is susceptible to H 2 O, N 2 , O 2 , CO, and CO.
The film quality is significantly changed by CO 2 and the like. for that reason,
It is important to be interested in the amount of impurity gas in the sputtering chamber.
【０００６】例えば、半導体基板上にＡｌ薄膜をスパッ
タリング法で形成する場合、スパッタ室内の残留ガスの
測定には、質量分析計が一般に使用される。しかし、ス
パッタリング中のＡｒガス中に混入する不純物ガス（Ｈ
2 Ｏ，Ｎ2 ，Ｏ2 ，ＣＯ，ＣＯ2 等）は、数１０ｐｐｍ
オ−ダで混入する。そのため、質量分析計の扱いが難し
く、製造中に絶えず測定するのは事実上不可能である。For example, when an Al thin film is formed on a semiconductor substrate by a sputtering method, a mass spectrometer is generally used for measuring a residual gas in a sputtering chamber. However, the impurity gas (H
2 O, N 2 , O 2 , CO, CO 2, etc.)
Mix in order. As a result, mass spectrometers are difficult to handle and virtually impossible to measure continuously during manufacture.
【０００７】このような理由から、製造工程における金
属薄膜の形成方法は、次のようにしている。 １．スパッタリング装置のメンテナンスをしする。 ２．用意したテストピ−スに薄膜を形成する。 ３．形成された薄膜の物性を測定する。 ４．３の測定で、基準を満たしていれば量産製造を開始
し、基準以下であれば１から再び繰り返す。 ここで、製造工程では正否の判定を素早くするため、３
の薄膜の物性はフ−プ硬度（Ｈｋ）、比抵抗（ρ）から
経験的に判定される。又、これらの物性値の判定からス
パッタ室内の不純物量、及び形成過程が正常であるかど
うかを判定している。For these reasons, a method of forming a metal thin film in a manufacturing process is as follows. 1. Maintain the sputtering equipment. 2. A thin film is formed on the prepared test piece. 3. The physical properties of the formed thin film are measured. In the measurement in 4.3, if the standard is satisfied, mass production is started, and if it is below the standard, the process is repeated from 1 again. Here, in the manufacturing process, in order to quickly determine the right or wrong, 3
The physical properties of the thin film are determined empirically from the Hoop hardness (Hk) and the specific resistance (ρ). Further, from the determination of these physical properties, the amount of impurities in the sputtering chamber and whether or not the formation process is normal are determined.
【０００８】しかし、これらの物性値は、薄膜の微小な
構造、即ち結晶粒界に析出する不純物量に対して鈍感で
あり、膜質の正確な指標になり得ない。そのため、半導
体装置の配線工程が全て完了した後、一定期間毎に金属
配線の電気的特性を調べている。電気的特性は、半導体
基板内の全チップを検査し統計処理を行うため１／３日
程度必要となる。その間、製造ラインは停止されてい
る。そして、電気的特性が基準内であれば製造開始とな
るが、基準以下であれば、前回の検査時から製造された
半導体装置が無駄となる。However, these physical values are insensitive to the minute structure of the thin film, that is, the amount of impurities precipitated at the crystal grain boundaries, and cannot be an accurate index of the film quality. Therefore, after all the wiring steps of the semiconductor device are completed, the electrical characteristics of the metal wiring are checked at regular intervals. The electrical characteristics require about one-third of a day to inspect all chips in the semiconductor substrate and perform statistical processing. Meanwhile, the production line has been shut down. If the electrical characteristics are within the standard, the production is started. If the electric characteristic is below the standard, the semiconductor device manufactured from the previous inspection is wasted.
【０００９】[0009]
【発明が解決しようとする課題】上述のように、従来、
金属薄膜の真の膜質は配線工程が完了しなければ測定で
きない。また、その測定に１／３日、即ち８時間程度か
かり、その間製造ラインが停止するため稼働率がわる
く、ある一定期間をもって検査するため生産性のロスに
つながる。従って、製造ラインが開始される前に行われ
る、テストピ−スを使った物性値の測定段階において、
真の膜質をしることが望まれる。As described above, conventionally,
The true quality of the metal thin film cannot be measured unless the wiring process is completed. In addition, the measurement takes 1/3 day, that is, about 8 hours, during which time the production line is stopped, the operation rate is deteriorated, and the inspection is performed in a certain period, which leads to a loss of productivity. Therefore, at the stage of measuring physical properties using a test piece, which is performed before the production line is started,
It is desirable to have true film quality.
【００１０】それ故、本発明は、金属薄膜の膜質を早期
に、簡単かつ正確に測定することにより、製造する際に
膜質がよい金属薄膜の形成方法を提供し、稼働率及び生
産性の向上を目的とする。Therefore, the present invention provides a method of forming a metal thin film having good film quality at the time of manufacturing by measuring the film quality of the metal thin film early, easily and accurately, thereby improving the operation rate and productivity. With the goal.
【００１１】[0011]
【課題を解決するための手段】半導体基板上に金属薄膜
がスパッタされ、該金属薄膜が形成された半導体基板が
熱処理される。その際、上記金属薄膜に内部応力が発生
する。その後、半導体基板を一定温度に保ち、上記内部
応力の緩和時間を測定する。内部応力は半導体基板の反
り量から測定する。A thin metal film is sputtered on a semiconductor substrate, and the semiconductor substrate on which the thin metal film is formed is subjected to a heat treatment. At that time, an internal stress is generated in the metal thin film. Thereafter, the semiconductor substrate is kept at a constant temperature, and the relaxation time of the internal stress is measured. The internal stress is measured from the amount of warpage of the semiconductor substrate.
【００１２】[0012]
【作用】半導体基板上に金属薄膜がスパッタされ熱処理
をされると、金属薄膜内に内部応力が発生する。該内部
応力は金属薄膜中の金属原子が自己拡散を生じ、徐々に
緩和される。内部応力緩和時間は、スパッタ中に金属薄
膜に混入した不純物量と関係がある。従って、内部応力
を測定することにより、スパッタ室内の残留ガス中の不
純物量が容易に判明するため、膜質の良い金属薄膜の形
成方法が提供できる。When a metal thin film is sputtered on a semiconductor substrate and subjected to heat treatment, internal stress is generated in the metal thin film. The internal stress causes self-diffusion of metal atoms in the metal thin film, and is gradually relaxed. The internal stress relaxation time is related to the amount of impurities mixed into the metal thin film during sputtering. Therefore, by measuring the internal stress, the amount of impurities in the residual gas in the sputtering chamber can be easily determined, so that a method for forming a metal thin film with good film quality can be provided.
【００１３】さらに、内部応力は半導体基板の反り量か
ら測定するため、短時間かつ簡便に金属薄膜の膜質がわ
かる。従って、金属薄膜に配線パタ−ンを形成する前の
段階において膜質をわかるため、稼働率及び生産性よく
半導体装置が製造できる。Further, since the internal stress is measured from the amount of warpage of the semiconductor substrate, the quality of the metal thin film can be easily determined in a short time. Therefore, the film quality can be determined before the wiring pattern is formed on the metal thin film, so that a semiconductor device can be manufactured with high operation rate and productivity.
【００１４】[0014]
【実施例】本発明をシリコン半導体基板への配線用Ａｌ
薄膜の形成方法を例に説明する。シリコン基板１１は、
（１１１）面のものを用いる。シリコン半導体基板上に
厚さ１．０μｍのＡｌ薄膜１３（但し、Ａｌ中にＳｉが
１ｗｔ％含有される）をスパッタリング法で形成する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention relates to an Al for wiring to a silicon semiconductor substrate.
A method for forming a thin film will be described as an example. The silicon substrate 11
A (111) plane is used. An Al thin film 13 having a thickness of 1.0 μm (1 wt% of Si is contained in Al) is formed on a silicon semiconductor substrate by a sputtering method.
【００１５】ここで、同一構造のシリコン基板を
（Ａ），（Ｂ），（Ｃ）３枚用意する。それら３枚の基
板は、金属薄膜が形成される際の条件が異なる。つまり
スパッタ室内の総不純物ガス量（Ｈ2 Ｏ，Ｎ2 ，Ｏ2 ，
ＣＯ，ＣＯ2 等）が異なり、（Ａ）は３０ｐｐｍ以下、
（Ｂ）は４５０ｐｐｍ、（Ｃ）は９００ｐｐｍの不純物
ガス量を含むスパッタ室内において、金属薄膜が形成さ
れる。Here, three silicon substrates (A), (B) and (C) having the same structure are prepared. These three substrates have different conditions when a metal thin film is formed. That is, the total impurity gas amount (H 2 O, N 2 , O 2 ,
CO, CO 2 etc.), (A) is 30 ppm or less,
A metal thin film is formed in a sputtering chamber containing an impurity gas amount of 450 ppm in (B) and 900 ppm in (C).
【００１６】まず、図１に示すように、シリコン基板１
１とＡｌ薄膜１３との反応を抑制するため、シリコン基
板１１に１０００オングストロ−ムのＳｉＯ2 膜１２を
形成する。このＳｉＯ2 膜１２はシリコン基板１１の表
裏対象に形成されるため、力学的には釣り合った状態で
ある。次に、シリコン基板１１表面にＡｌ薄膜１３をス
パッタする。その後、シリコン基板１１は４５０℃で３
０分間Ｎ2 雰囲気中で熱処理をされる。熱処理中に発生
するＡｌ膜１３中の内部応力の経時変化を、２００℃に
保った状態で測定する。内部応力はシリコン基板１１の
反り量から求める。該反り量は、シリコン基板１１の裏
面の端部を結ぶ水平面の中心と、該中心からの垂直方向
上にあるシリコン基板１１の裏面を結ぶ距離ｄ（図２）
によって表される。First, as shown in FIG.
In order to suppress the reaction between 1 and the Al thin film 13, a 1000 Å SiO 2 film 12 is formed on the silicon substrate 11. Since this SiO 2 film 12 is formed on the front and back of the silicon substrate 11, it is in a mechanically balanced state. Next, an Al thin film 13 is sputtered on the surface of the silicon substrate 11. After that, the silicon substrate 11
Heat treatment is performed in an N 2 atmosphere for 0 minutes. The change with time of the internal stress in the Al film 13 generated during the heat treatment is measured while maintaining the temperature at 200 ° C. The internal stress is determined from the amount of warpage of the silicon substrate 11. The amount of warpage is determined by a distance d (FIG. 2) connecting the center of the horizontal plane connecting the ends of the back surface of the silicon substrate 11 and the back surface of the silicon substrate 11 vertically above the center.
Represented by
【００１７】図３に、（Ａ），（Ｂ），（Ｃ）の時間−
応力特性を示す。（Ａ），（Ｂ），（Ｃ）には明らかな
差が現れている。つまり、スパッタ室内の不純物ガス量
が少ない程、急激に応力が緩和されており、緩和に要す
る時間はスパッタ室内の不純物ガス量に大きく依存して
いる。なぜなら、スパッタの際にＡｌ薄膜１３中に室内
の不純物が取り込まれ、熱処理によりＡｌ薄膜１３中に
引張応力が生じるからである。その際、生じた応力はＡ
ｌ原子の自己拡散により緩和されるが、不純物量に比例
して応力の緩和が遅れるのは、Ａｌ原子の自己拡散がＡ
ｌ薄膜１３中に取り込まれた不純物に疎外されるためと
考えられる。FIG. 3 shows time (A), (B) and (C).
Shows stress characteristics. (A), (B), and (C) show a clear difference. That is, as the amount of the impurity gas in the sputtering chamber is smaller, the stress is relieved sharply, and the time required for the relaxation largely depends on the amount of the impurity gas in the sputtering chamber. This is because impurities in the chamber are taken into the Al thin film 13 during sputtering, and a tensile stress is generated in the Al thin film 13 by the heat treatment. At that time, the generated stress is A
Although the relaxation of the stress is delayed in proportion to the amount of impurities, the self-diffusion of Al
This is considered to be due to the alienation of impurities taken into the thin film 13.
【００１８】ところで、Ａｌ薄膜１３の膜質はＡｌ中の
結晶粒界に折出する不純物量に影響される。従って、金
属薄膜の内部応力を測定することにより、金属薄膜の膜
質まで判明できる。Incidentally, the film quality of the Al thin film 13 is affected by the amount of impurities protruding to crystal grain boundaries in Al. Therefore, by measuring the internal stress of the metal thin film, the quality of the metal thin film can be determined.
【００１９】また、図４は試料の応力緩和速度が１×１
０7 dyne／cm2 ・分以下になるまでの時間と試料の高温
放置試験寿命（ＭＴＴＦ：Ｍｅａｎ Ｔｉｍｅ ｔｏＦ
ａｉｌ）の関係を示す。図３と図４中のａ，ｂ，ｃはそ
れぞれ対応している。ａは試料（Ａ）において応力緩和
速度が１×１０7 dyne／cm2 ・分の点を示しており、
ｂ，ｃも同様である。図２より、寿命２０００Ｈを補償
するには、応力緩和時間は１５分以下、寿命１５００Ｈ
の補償には１７分以下であれば良いことになる。FIG. 4 shows that the stress relaxation rate of the sample is 1 × 1.
0 7 dyne / cm 2 The time until the temperature becomes less than minutes and the high temperature storage test life of the sample (MTTF: Mean Time to F)
aile). A, b, and c in FIGS. 3 and 4 correspond to each other. a is the sample (A) having a stress relaxation rate of 1 × 10 7 dyne / cm 2 ・ It shows the minute point,
The same applies to b and c. As shown in FIG. 2, in order to compensate for the life of 2000H, the stress relaxation time is 15 minutes or less and the life is 1500H.
Will be sufficient if it is 17 minutes or less.
【００２０】以上より、測定の所要時間は２０〜３０分
程度で十分である。その上、半導体基板の反り量により
内部応力を求めるだけで膜質まで判明する。従って、従
来金属薄膜の物性値を測定する際に、物性値ではなく膜
質まで測定することにより、金属薄膜の製造工程の早期
に、スパッタ室内の不純物ガス量が簡便にわかりことが
できる。同様の応力緩和現象はＡｌ以外の材料でも、測
定時の保持温度によって起こるのは自明であり、材料の
異なる薄膜の膜質の測定にも使用できる。From the above, it is sufficient that the time required for the measurement is about 20 to 30 minutes. In addition, the film quality can be determined only by obtaining the internal stress based on the amount of warpage of the semiconductor substrate. Therefore, by measuring not the physical property value but the film quality when measuring the physical property value of the conventional metal thin film, the amount of the impurity gas in the sputtering chamber can be easily determined at an early stage of the manufacturing process of the metal thin film. It is obvious that the same stress relaxation phenomenon occurs with materials other than Al depending on the holding temperature at the time of measurement, and the stress relaxation phenomenon can be used for measuring the film quality of thin films made of different materials.
【００２１】[0021]
【発明の効果】本発明によれば、金属薄膜中の内部応力
の緩和時間から膜質を判定し、これを膜形成工程にフィ
−ドバックして膜質を制御できる。内部応力は半導体基
板の反り量から測定するため、容易に行える。従来、金
属薄膜に配線パタ−ンを形成した後でなければ、金属薄
膜の膜質が測定できずにいた。しかし、内部応力を測定
することにより、従来の物性値を測定する段階におい
て、膜質まで測定できる。従って、金属薄膜の製造工程
の早期に、スパッタ室内の不純物ガス量が簡便にわかる
ため、良質の金属薄膜が形成され、稼働率及び生産性よ
く半導体装置が製造できる。According to the present invention, the film quality can be determined by judging the film quality from the relaxation time of the internal stress in the metal thin film and feeding it back to the film forming step. The internal stress is easily measured because it is measured from the amount of warpage of the semiconductor substrate. Conventionally, the quality of a metal thin film cannot be measured unless a wiring pattern is formed on the metal thin film. However, by measuring the internal stress, it is possible to measure even the film quality at the stage of measuring the conventional physical property values. Therefore, since the amount of impurity gas in the sputtering chamber can be easily determined at an early stage of the metal thin film manufacturing process, a high-quality metal thin film is formed, and a semiconductor device can be manufactured with high operation rate and productivity.
【図１】本発明の実施例において、基板上に金属薄膜が
被着した状態を示す断面図である。FIG. 1 is a cross-sectional view showing a state in which a metal thin film is deposited on a substrate in an embodiment of the present invention.
【図２】本発明の実施例において、基板の反りを示す断
面図である。FIG. 2 is a cross-sectional view showing a warpage of a substrate in the example of the present invention.
【図３】本発明による時間に対する応力の変化の図であ
る。FIG. 3 is a diagram of the change in stress over time according to the present invention.
【図４】本発明による応力緩和時間に対する高温放置試
験寿命の変化の図である。FIG. 4 is a graph showing a change in a high-temperature storage test life with respect to a stress relaxation time according to the present invention.
１１…シリコン基板，１２…ＳｉＯ2 膜，１３…Ａｌ薄
膜11: silicon substrate, 12: SiO 2 film, 13: Al thin film
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 33/00 G01N 25/00 H01L 21/66 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 7 , DB name) G01N 33/00 G01N 25/00 H01L 21/66
Claims (7)
を不活性雰囲気中で第１の温度で熱処理し、熱処理中に
生じる上記金属薄膜の内部応力を、上記第１の温度より
低い第２の温度で測定することを特徴とする金属薄膜の
膜質の測定方法。After depositing a metal thin film on a substrate, the substrate is heat-treated at a first temperature in an inert atmosphere, and the internal stress of the metal thin film generated during the heat treatment is reduced from the first temperature. A method for measuring the quality of a metal thin film, wherein the measurement is performed at a low second temperature.
シリコン基板であることを特徴とする請求項１記載の金
属薄膜の膜質の測定方法。2. The method according to claim 1, wherein the substrate is a silicon substrate having SiO 2 films on both surfaces.
れることを特徴とする請求項１記載の金属薄膜の膜質の
測定方法。3. The method for measuring the quality of a metal thin film according to claim 1, wherein the metal thin film is applied by a sputtering method.
り量により求めることを特徴とする請求項１記載の金属
薄膜の膜質の測定方法。4. The method for measuring the quality of a metal thin film according to claim 1, wherein the internal stress of the metal thin film is obtained from the amount of warpage of the substrate.
特徴とする請求項１記載の金属薄膜の膜質の測定方法。5. The method for measuring the quality of a metal thin film according to claim 1, wherein the first temperature is 450 ° C.
特徴とする請求項１記載の金属薄膜の膜質の測定方法。6. The method for measuring the quality of a metal thin film according to claim 1, wherein the second temperature is 200 ° C.
用金属として用いられるＡｌまたはＡｌ合金であること
を特徴とする請求項１記載の金属薄膜の膜質の測定方
法。7. The method according to claim 1, wherein said metal thin film is Al or an Al alloy used as a wiring metal in a semiconductor device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04070633A JP3107638B2 (en) | 1992-03-27 | 1992-03-27 | Measuring method of metal thin film quality |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04070633A JP3107638B2 (en) | 1992-03-27 | 1992-03-27 | Measuring method of metal thin film quality |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05273201A JPH05273201A (en) | 1993-10-22 |
| JP3107638B2 true JP3107638B2 (en) | 2000-11-13 |
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ID=13437244
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP04070633A Expired - Fee Related JP3107638B2 (en) | 1992-03-27 | 1992-03-27 | Measuring method of metal thin film quality |
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| JP (1) | JP3107638B2 (en) |
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|---|---|---|---|---|
| JP7546272B2 (en) * | 2020-05-07 | 2024-09-06 | 株式会社ブイ・テクノロジー | Tension measuring device and tension measuring method |
| CN115424950B (en) * | 2022-08-04 | 2023-10-20 | 淮安澳洋顺昌光电技术有限公司 | Method for testing stress of metal film |
| CN120558163B (en) * | 2025-07-30 | 2025-10-21 | 圆周率半导体(南通)有限公司 | PCB warp detection method and system |
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- 1992-03-27 JP JP04070633A patent/JP3107638B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05273201A (en) | 1993-10-22 |
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