JPS629667B2 - - Google Patents
Info
- Publication number
- JPS629667B2 JPS629667B2 JP57119913A JP11991382A JPS629667B2 JP S629667 B2 JPS629667 B2 JP S629667B2 JP 57119913 A JP57119913 A JP 57119913A JP 11991382 A JP11991382 A JP 11991382A JP S629667 B2 JPS629667 B2 JP S629667B2
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- nitride thin
- nitrogen
- resistivity
- hydrogen
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
Description
【発明の詳細な説明】
本発明は、内部応力が小さく、かつ比抵抗の少
い金属窒化物の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing a metal nitride with low internal stress and low specific resistance.
一般にチタン、モリブデン、タンタル等の高融
点金属の窒化物は、きわめて高い融点と高い機械
的硬度を有し、熱的・化学的にも安定であるため
に、各種装置・部品の機械的・熱的保護膜として
使用され、最近ではさらに半導体集積回路の高耐
熱電極材料の一つとして実用化されつつある。 In general, nitrides of high-melting point metals such as titanium, molybdenum, and tantalum have extremely high melting points and high mechanical hardness, and are thermally and chemically stable. It is used as a protective film, and recently it is being put into practical use as a highly heat-resistant electrode material for semiconductor integrated circuits.
金属窒化物薄膜を半導体集積回路の電極材料と
して用いる場合、比抵抗が低いことが第１の条件
である。 When using a metal nitride thin film as an electrode material for a semiconductor integrated circuit, the first condition is that the specific resistance is low.
一般に、チタン、ジルコニウムなどの窒化物は
バルクで比較すると、もとの金属元素よりも比抵
抗が小さくなることが知られている。しかし、電
極材料に用いる厚さ数100〜数1000Åの薄膜で
は、種々の散乱機構のために比抵抗は一般に高く
なる傾向があり、これを下げることが一つの重要
な技術となつている。 Generally, it is known that nitrides such as titanium and zirconium have a lower resistivity than the original metal element when compared in bulk. However, thin films used as electrode materials with a thickness of several hundred to several thousand angstroms generally tend to have a high specific resistance due to various scattering mechanisms, and reducing this resistance is an important technique.
例えば、窒化チタン薄膜を窒素・アルゴン混合
ガス中の反応性スパツタリングにより得る場合、
窒素分圧、窒素・アルゴン混合ガス圧力を増加さ
せると窒化チタン薄膜の元素組成、膜中の不純物
の影響により比抵抗は増加するため、通常は放電
が持続できる最小の圧力に設定される。また、さ
らに比抵抗を下げるために基板に負の直流バイア
ス電圧を印加することが効果的である。 For example, when a titanium nitride thin film is obtained by reactive sputtering in a nitrogen/argon mixed gas,
When the nitrogen partial pressure or the nitrogen/argon mixed gas pressure is increased, the resistivity increases due to the elemental composition of the titanium nitride thin film and impurities in the film, so it is usually set to the minimum pressure that can sustain discharge. Furthermore, it is effective to apply a negative DC bias voltage to the substrate in order to further lower the resistivity.
第１図は、基板に負のバイアス電圧を印加した
スパツタリング装置の概略図を示すものであり、
図において１は真空チヤンバ、２は排気系、３は
チタン、モリブデン、タンタル等の金属ターゲツ
ト、４はしやへい板、５は高周波電源回路、６は
基板、７はバイアス電源、８はガス導入口、９は
流量調節弁である。第２図は窒化チタン薄膜の場
合の膜の比抵抗（白丸）と膜内に発生した内部応
力（黒丸）について、基板バイアスの効果を示し
たグラフである。縦軸のρは比抵抗、σは内部応
力、横軸ＶBはバイアス電圧を示す。このデータ
は窒素分圧2.8ｍTorr、窒素・アルゴン混合ガス
圧力16.8ｍTorr、高周波電力400Wの場合であ
る。 FIG. 1 shows a schematic diagram of a sputtering apparatus in which a negative bias voltage is applied to a substrate.
In the figure, 1 is a vacuum chamber, 2 is an exhaust system, 3 is a metal target such as titanium, molybdenum, tantalum, etc., 4 is a shield plate, 5 is a high frequency power supply circuit, 6 is a substrate, 7 is a bias power supply, and 8 is a gas introduction The port and 9 are flow control valves. FIG. 2 is a graph showing the effect of substrate bias on the specific resistance of a titanium nitride thin film (white circles) and the internal stress generated within the film (black circles). On the vertical axis, ρ indicates specific resistance, σ indicates internal stress, and horizontal axis V B indicates bias voltage. This data is for a nitrogen partial pressure of 2.8 mTorr, a nitrogen/argon mixed gas pressure of 16.8 mTorr, and a high frequency power of 400 W.
このように、基板バイアス印加は窒化チタン薄
膜の比抵抗の低減に対してきわめて効果的ではあ
るが、反面膜内に著しい内部応力σが発生するた
め、半導体集積回路を製造する際にウエハのそり
により微細パターンの形成が困難となること、膜
が厚いい場合にはクラツクやはがれが発生するな
ど著しい障害の原因となつていた。 In this way, applying a substrate bias is extremely effective in reducing the resistivity of titanium nitride thin films, but on the other hand, it generates significant internal stress σ within the film, which can cause wafer warpage during the manufacture of semiconductor integrated circuits. This makes it difficult to form fine patterns, and when the film is thick, it causes serious problems such as cracking and peeling.
本発明は、以上の問題を解決するために、窒
素・アルゴン混合ガス中にさらに水素を添加し、
基板に直流バイアスを印加することなしに、金属
窒化物薄膜の比抵抗を実用上問題ないレベルにま
で下げることを目的とするものである。 In order to solve the above problems, the present invention further adds hydrogen to the nitrogen/argon mixed gas,
The purpose of this method is to lower the resistivity of a metal nitride thin film to a level that does not pose any practical problems without applying a DC bias to the substrate.
前記の目的を達成するため、本発明は導電性を
有する金属窒化物薄膜を反応性スパツタ法で形成
する金属窒化物薄膜の製造方法において、窒素、
アルゴン混合ガスに水素を添加した雰囲気で形成
することを特徴とする金属窒化物薄膜の製造方法
を発明の要旨とするものである。 In order to achieve the above object, the present invention provides a method for producing a metal nitride thin film having conductivity by a reactive sputtering method.
The gist of the invention is a method for producing a metal nitride thin film, which is characterized in that it is formed in an atmosphere in which hydrogen is added to an argon mixed gas.
次に本発明の実施例を添附図面について説明す
る。なお実施例は一つの例示であつて、本発明の
精神を逸脱しない範囲内で、種々の変更あるいは
改良を行いうることは云うまでもない。 Next, embodiments of the present invention will be described with reference to the accompanying drawings. It should be noted that the embodiments are merely illustrative, and it goes without saying that various changes and improvements can be made without departing from the spirit of the present invention.
本発明の実施に用いられる装置は、第１図に示
すものであり、手順はまずチヤンバ１内を排気
後、水素をガス導入口８に設けられた流量調節弁
９を調節することにより、所定の分圧になるまで
導入する。つづいて窒素を水素の分圧との和が所
定の圧力になる様に導入し、最後にアルゴンを全
圧力が所定の圧力となるまで導入したのち、放電
を開始させ、金属窒化物薄膜を堆積させる。この
とき基板バイアスは本発明の主旨からすれば、必
ずしも必要でないが、印加することは可能であ
る。 The apparatus used to carry out the present invention is shown in FIG. 1, and the procedure is to first exhaust the inside of the chamber 1, and then supply hydrogen to a predetermined level by adjusting the flow rate control valve 9 provided at the gas inlet 8. Introduce until the partial pressure reaches . Next, nitrogen is introduced so that the sum of the partial pressure of hydrogen becomes the predetermined pressure, and finally, argon is introduced until the total pressure reaches the predetermined pressure, then discharge is started and a metal nitride thin film is deposited. let At this time, a substrate bias is not necessarily required in view of the gist of the present invention, but it is possible to apply it.
第３図は一例として、窒化チタン薄膜を窒素分
圧2.8ｍTorr、窒素・アルゴン混合ガス圧力を、
16.8ｍTorr、高周波電力400Wとし、窒素・アル
ゴン混合ガス中にさらに水素を窒素に対する分圧
比すなわちＰH／ＰNが０、0.5および１と変化さ
せて加えた場合に堆積した窒化チタン薄膜の比抵
抗の基板バイアス依存性を示したものであり、第
４図は同様に内部応力の水素添加の効果および基
板バイアス依存性を示したものである。第３図お
よび第４図から、著しい内部応力が発生しない基
板バイアスの範囲内で、水素添加により実用上十
分な値にまで比抵抗を下げることが可能であるこ
とを示している。この場合、基板バイアスをわず
かに印加することは、基板バイアスを全く印加し
ない場合よりも比抵抗を下げることに有効である
が、水素添加の効果は基板バイアスが無い場合に
もあり、十分その目的は達成される。添加すべき
水素の量は分圧比ＰH／ＰNで１〜２が最適であ
り、これを越えると比抵抗は再び増加することが
示された。第５図はそのデータの一例を示すもの
であり、分圧比１〜２に比抵抗の最小値が存在す
る。 As an example, Figure 3 shows a titanium nitride thin film at a nitrogen partial pressure of 2.8 mTorr and a nitrogen/argon mixed gas pressure.
Specific resistance of the titanium nitride thin film deposited when hydrogen was added to the nitrogen/argon mixed gas at 16.8 mTorr and high frequency power of 400 W, with the partial pressure ratio to nitrogen, that is, P H /P N , varied from 0, 0.5, and 1. FIG. 4 similarly shows the effect of hydrogen addition and the dependence of internal stress on substrate bias. FIGS. 3 and 4 show that it is possible to lower the resistivity to a practically sufficient value by adding hydrogen within the substrate bias range where significant internal stress does not occur. In this case, applying a slight substrate bias is more effective in lowering the resistivity than applying no substrate bias at all, but the effect of hydrogenation is also present in the absence of a substrate bias, and is sufficient for its purpose. is achieved. It has been shown that the optimal amount of hydrogen to be added is a partial pressure ratio of 1 to 2, P H /P N , and that when this is exceeded, the resistivity increases again. FIG. 5 shows an example of the data, and the minimum value of resistivity exists at a partial pressure ratio of 1 to 2.
以上説明したように、本発明によれば反応性ス
パツタリングにおいて窒素・アルゴン混合ガス中
に水素を添加することにより、内部応力が小さ
く、比抵抗の小さな金属窒化物薄膜を容易に得る
ことができ、この薄膜を半導体集積回路の電極の
一部に、例えば拡散障壁層として使用すれば、耐
熱性ならびに信頼性に優れた半導体集積回路が歩
留り良く、経済的に実現することができる。 As explained above, according to the present invention, by adding hydrogen to a nitrogen/argon mixed gas in reactive sputtering, a metal nitride thin film with low internal stress and low resistivity can be easily obtained. If this thin film is used as a part of an electrode of a semiconductor integrated circuit, for example, as a diffusion barrier layer, a semiconductor integrated circuit with excellent heat resistance and reliability can be economically realized with high yield.
なお水素添加により比抵抗が低減される機構と
しては、金属窒化物薄膜中に含まれ、かつ比抵抗
を増加させると考えられる酸素の膜中への混入
を、その強力な還元作用により抑制することが考
えられる。 The mechanism by which the resistivity is reduced by hydrogen addition is that its strong reducing action suppresses the incorporation of oxygen, which is contained in the metal nitride thin film and is thought to increase the resistivity, into the film. is possible.
第１図はスパツタリング装置の概略図、第２図
は窒化チタン薄膜を高周波反応性スパツタリング
法により形成した場合の膜の比抵抗と内部応力に
ついて基板バイアス効果を示すグラフ、第３図は
水素・窒素・アルゴン混合ガス中で同じく形成し
た窒化チタン薄膜の比抵抗の基板バイアスおよび
水素添加量の効果を示すグラフ、第４図は同じく
内部応力の基板バイアスおよび水素添加量の効果
を示すグラフ、第５図は水素・窒素の分圧比を変
化させたときの比抵抗に最小値が存在することを
示すグラフである。
１……真空チヤンバ、２……排気系、３……金
属ターゲツト、４……しやへい板、５……高周波
電源回路、６……基板、７……バイアス電源、８
……ガス導入口、９……流量調節弁。
Figure 1 is a schematic diagram of the sputtering equipment, Figure 2 is a graph showing the substrate bias effect on the specific resistance and internal stress of a titanium nitride thin film formed by high-frequency reactive sputtering, and Figure 3 is a graph showing the substrate bias effect on the specific resistance and internal stress of a titanium nitride thin film formed by high-frequency reactive sputtering.・A graph showing the effect of substrate bias and amount of hydrogen addition on the resistivity of a titanium nitride thin film similarly formed in an argon mixed gas. Figure 4 is a graph showing the effect of substrate bias and amount of hydrogen addition on internal stress. The figure is a graph showing that there is a minimum value in specific resistance when the partial pressure ratio of hydrogen and nitrogen is changed. 1... Vacuum chamber, 2... Exhaust system, 3... Metal target, 4... Shrink plate, 5... High frequency power supply circuit, 6... Substrate, 7... Bias power supply, 8
...Gas inlet, 9...Flow control valve.
Claims (1)
ツタ法で形成する金属窒化物薄膜の製造方法にお
いて、窒素、アルゴン混合ガス中で窒素に対する
分圧比が0.5乃至２の水素を添加した雰囲気で形
成することを特徴とする金属窒化物薄膜の製造方
法。1. In a method for manufacturing a metal nitride thin film having conductivity by a reactive sputtering method, the metal nitride thin film is formed in a mixed gas of nitrogen and argon in an atmosphere to which hydrogen is added at a partial pressure ratio of 0.5 to 2 to nitrogen. A method for producing a metal nitride thin film, characterized by the following.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11991382A JPS5913607A (en) | 1982-07-12 | 1982-07-12 | Manufacture of thin metallic nitride film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11991382A JPS5913607A (en) | 1982-07-12 | 1982-07-12 | Manufacture of thin metallic nitride film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5913607A JPS5913607A (en) | 1984-01-24 |
| JPS629667B2 true JPS629667B2 (en) | 1987-03-02 |
Family
ID=14773287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11991382A Granted JPS5913607A (en) | 1982-07-12 | 1982-07-12 | Manufacture of thin metallic nitride film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5913607A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04365965A (en) * | 1991-06-12 | 1992-12-17 | Toyota Autom Loom Works Ltd | Protecting device for engine |
| JPH086098Y2 (en) * | 1991-08-07 | 1996-02-21 | 日本機械工業株式会社 | Inclined slide type scour prevention device |
| JP2565086Y2 (en) * | 1991-08-08 | 1998-03-11 | 日本機械工業株式会社 | Inclined slide scour prevention device |
| EP0576376B1 (en) * | 1992-06-26 | 1998-05-06 | Eastman Kodak Company | Cobalt platinum magnetic film and method of fabrication thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5428390A (en) * | 1977-08-05 | 1979-03-02 | Kuraray Co Ltd | Preparation of modified polyvinyl alcohol-type polymer |
-
1982
- 1982-07-12 JP JP11991382A patent/JPS5913607A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5913607A (en) | 1984-01-24 |
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