JP2000199065A - Formation of coating film of carbon or essentially consisting of carbon - Google Patents
Formation of coating film of carbon or essentially consisting of carbonInfo
- Publication number
- JP2000199065A JP2000199065A JP36989899A JP36989899A JP2000199065A JP 2000199065 A JP2000199065 A JP 2000199065A JP 36989899 A JP36989899 A JP 36989899A JP 36989899 A JP36989899 A JP 36989899A JP 2000199065 A JP2000199065 A JP 2000199065A
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- forming
- reaction chamber
- film
- main component
- 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.)
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Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、炭素または炭素を
主成分とする被膜を形成する装置のクリーニング方法に
関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for cleaning an apparatus for forming a coating containing carbon or carbon as a main component.
【0002】[0002]
【従来の技術】炭素膜は、従来より耐摩耗性、高平滑
性、絶縁性及び耐薬品性等に優れており、多くの特性を
有する材料としてその応用が期待されており、その炭素
膜をコーティングする技術としては、特開昭56-146930
号公報が知られている。2. Description of the Related Art Conventionally, carbon films are superior in wear resistance, high smoothness, insulating properties and chemical resistance, and are expected to be applied as materials having many characteristics. As a coating technique, Japanese Patent Application Laid-Open No. 56-146930
A gazette is known.
【0003】しかし、同一反応器による複数回の成膜
は、真空度の低下、フレークの問題等により困難であり
1回ないし2回成膜後は、反応器内部のクリーニングが
必要となる。従来のクリーニングに用いられる気体は、
固体被膜の成分から、例えば炭素系であればプラズマ反
応によって揮発性ガスとする為、水素、酸素、弗化物気
体があげられる。However, it is difficult to form a film a plurality of times in the same reactor due to a decrease in the degree of vacuum, a problem of flakes, and the like. After forming the film once or twice, the inside of the reactor needs to be cleaned. The gas used for conventional cleaning is
From the components of the solid coating, for example, hydrogen, oxygen, and fluoride gases are used in the case of a carbon-based material in order to generate a volatile gas by a plasma reaction.
【0004】[0004]
【発明が解決しようとする課題】炭素膜または炭素膜を
主成分とする被膜をエッチングする技術は、炭素膜を応
用する上で大きな問題となっている。例えば、エッチン
グの際水素を用いて炭素膜と反応させCxHy等を生じさ
せる炭化水素系ガス化反応を行わせる方法は、反応器内
の汚染は低減されるが、エッチング速度が遅く量産性の
面で問題が多い。The technique of etching a carbon film or a film containing a carbon film as a main component is a major problem in applying a carbon film. For example, a method of causing a hydrocarbon gasification reaction to produce a C x H y or the like is reacted with carbon film with hydrogen during the etching, although the contamination in the reactor is reduced, the etching speed slower mass There are many problems in terms of gender.
【0005】一方、炭素膜のプラズマエッチングに用い
るガスとしては、O2が最も簡便で揮発性ガス化反応に
よりCO、CO2等として排気されるものが大部分であ
るが、未反応の壁でO、O2あるいはCO、CO2として
反応室内壁に吸着し、クリーニング後に成膜する際それ
らが内壁から離脱し、気相中にアウトディフェージョン
し、膜内にオートドーピングあるいは界面にトラップさ
れ、膜質、界面特性(主に密着性)を低下させる原因と
なっていた。On the other hand, most of the gases used for plasma etching of the carbon film are those in which O 2 is the simplest and is exhausted as CO, CO 2, etc. by a volatile gasification reaction. O, O 2 or CO, CO 2 is adsorbed on the inner wall of the reaction chamber as a film, and when forming a film after cleaning, they are separated from the inner wall, out-phase in the gas phase, and are auto-doped in the film or trapped at the interface , Film quality and interface characteristics (mainly adhesion).
【0006】[0006]
【課題を解決するための手段】本発明は上記の問題を解
決する為に従来のエッチングガスによる反応容器内部の
基体、または基板等の被膜成形面以外に堆積している炭
素系被膜の除去後に不活性ガス、例えばArまたは活性
ガス、例えばH2によるプラズマクリーニング処理を行
ない、内壁に残存しているO、O2、CO、CO2等を除
去または置換することにより、反応室内を清浄化するこ
とを特徴とする。SUMMARY OF THE INVENTION In order to solve the above-mentioned problems, the present invention provides a method for removing a carbon-based coating deposited on a substrate or a substrate other than a coating forming surface of a reaction vessel by a conventional etching gas. The inside of the reaction chamber is cleaned by performing a plasma cleaning process using an inert gas, for example, Ar or an active gas, for example, H 2 to remove or replace O, O 2 , CO, CO 2, etc. remaining on the inner wall. It is characterized by the following.
【0007】図1にエッチング用気体であるNF3、
H2、O2を用いてビッカース硬度1000kg/mm2及び2000k
g/mm2の硬質炭素膜をエッチングした場合のエッチング
速度及び高周波印加電極側に生じるセルフバイアスを示
した。FIG. 1 shows NF 3 , which is an etching gas,
Using H 2, O 2 Vickers hardness 1000 kg / mm 2 and 2000k
The etching rate and the self-bias generated on the high-frequency application electrode side when a g / mm 2 hard carbon film was etched are shown.
【0008】図中○は、セルフバイアスを表し、□はビ
ッカース硬度1000kg/mm2、◇はビッカース硬度2000kg
/mm2に対するエッチング速度を表す。この場合、高周
波エネルギーは60w、エッチング用気体の流量は50SC
CM、温度は室温、反応圧力は3Paで行った。In the figure, 図 represents self-bias, □ represents Vickers hardness of 1000 kg / mm 2 , Δ represents Vickers hardness of 2000 kg
/ Mm 2 represents the etching rate. In this case, the high-frequency energy is 60 W and the flow rate of the etching gas is 50 SC.
CM was carried out at room temperature and at a reaction pressure of 3 Pa.
【0009】次に本発明において、反応容器内部のエッ
チングとクリーニング及び置換方法についての組合せの
例を以下に示す。 〔1〕O2プラズマエッチング+Arプラズマクリーニ
ング 〔2〕NF3プラズマエッチング+Arプラズマクリー
ニング 〔3〕O2プラズマエッチング+H2プラズマクリーニン
グ 〔4〕NF3プラズマエッチング+H2プラズマクリーニ
ング 〔5〕H2プラズマエッチング+H2プラズマクリーニン
グNext, in the present invention, examples of combinations of etching, cleaning and replacement methods inside the reaction vessel will be described below. [1] O 2 plasma etching + Ar plasma cleaning [2] NF 3 plasma etching + Ar plasma cleaning [3] O 2 plasma etching + H 2 plasma cleaning [4] NF 3 plasma etching + H 2 plasma cleaning [5] H 2 plasma etching + H 2 Plasma cleaning
【0010】[0010]
【実施例】 以下に本発明を実施例に従って説明する。
図2に本発明の実施に使用した炭素または炭素を主成分
とする被膜をエッチング除去した後プラズマクリーニン
グするための平行平板形のプラズマ装置の概要を示す。EXAMPLES The present invention will be described below with reference to examples.
FIG. 2 shows an outline of a parallel plate type plasma apparatus for performing plasma cleaning after etching and removing carbon or a film containing carbon as a main component used in the present invention.
【0011】図面では、ガス系(1)においてキャリア
ガスである水素を(2)より、反応性気体である炭化水
素気体、例えばメタン、エチレンを(3)より、炭素膜
のエッチング用気体である弗化物気体、例えばNF3を
(3)より、またアルゴン、水素、酸素等のエッチング
及びクリーニング用気体を(4)よりバルブ(6)、流
量計(7)をへて反応系(8)中のノズル(9)より導
入する反応系(8)では、減圧下にて炭素膜の成膜また
は炭素膜のエッチング処理を行った。In the drawing, in the gas system (1), hydrogen as a carrier gas is a gas for etching a carbon film from (2), and a hydrocarbon gas as a reactive gas such as methane and ethylene is a gas from (3). A fluoride gas, for example, NF 3 from (3), and an etching and cleaning gas such as argon, hydrogen, oxygen, etc. from (4) through a valve (6) and a flow meter (7) into a reaction system (8). In the reaction system (8) introduced from the nozzle (9), a carbon film was formed or the carbon film was etched under reduced pressure.
【0012】反応室(8)では第1の電極(10)、第
2の電極(11)を有し、一対の電極(10)、(1
1)間には高周波電源(12)よりマッチングトランス
(13)、直流バイアス電源(14)より電気エネルギ
ーが加えられ、プラズマが発生する。The reaction chamber (8) has a first electrode (10) and a second electrode (11), and has a pair of electrodes (10), (1).
During 1), a high frequency power source (12) applies a matching transformer (13) and a DC bias power source (14) applies electric energy to generate plasma.
【0013】反応性気体のより一層の分析を行なうため
には、2.45GHzのマイクロ波にて200w〜2kwのマ
イクロ波励起(15)を与えてもよい。すると活性の反
応性気体の量を増やすことができ、例えば炭素系被膜の
酸素によるエッチング速度を約4倍に向上することがで
きた。In order to further analyze the reactive gas, a microwave excitation (15) of 200 w to 2 kW may be provided by a microwave of 2.45 GHz. As a result, the amount of the active reactive gas could be increased, and for example, the etching rate of the carbon-based film with oxygen could be improved about four times.
【0014】これらの反応性気体は、反応空間(16)
で0.01〜1Torr例えば0.1Torrとし、高周波による電磁
エネルギーにより50w〜5kwのエネルギーが加えられ
る。直流バイアスは、被膜形成面上に−200〜600v(実
質的には−400〜400v)を加えられる。なぜなら、直流
バイアスが零のときは、自己バイアスが−200v(第2
の電極を接地レベルとして)を有しているためである。These reactive gases form a reaction space (16).
To 0.01 Torr, for example, 0.1 Torr, and 50 w to 5 kW of energy is applied by electromagnetic energy of high frequency. A DC bias is applied to the film forming surface from -200 to 600 V (substantially -400 to 400 V). Because, when the DC bias is zero, the self-bias is -200 V (second
Is used as the ground level).
【0015】基板としてSiウェハを用いたものと、Al
の板に磁気記録媒体であるγFe2O3をつけたものとを
用いて本発明方法により反応室を清浄化した後、公知の
方法により図3に示すように炭素系被膜を成膜した。本
実施例では反応室の清浄化方法としてエッチング用気体
にH2プラズマのみを用いる方法とエッチング用気体に
O2プラズマのみを用いる方法と、エッチング用気体に
O2プラズマを用いその後にH2プラズマクリーニングす
る方法とを行った。A substrate using a Si wafer as a substrate and an Al substrate
After the reaction chamber was cleaned by the method of the present invention using γFe 2 O 3 , which is a magnetic recording medium, on the plate of No. 1 above, a carbon-based film was formed by a known method as shown in FIG. A method using only O 2 plasma process and an etching gas using only H 2 plasma etching gas as cleaning method of the reaction chamber in this embodiment, then in H 2 plasma using O 2 plasma etching gas Cleaning method was performed.
【0016】表1に成膜した炭素系被膜に対して粒径1
〜2μmのダイヤモンドペーストを使用したアブレシブ
テストを行った結果を示す。The particle size of the carbon-based film formed in Table 1 was 1
The results of an abrasive test using a diamond paste of 2 μm are shown.
【0017】評価は○、○△、△、△×、×の5段階で
おこなった。その結果、酸素プラズマエッチッグのみの
場合に比べて顕著な差が見られた。The evaluation was performed in five stages of ○, ○ △, Δ, Δ ×, ×. As a result, a remarkable difference was observed as compared with the case of using only the oxygen plasma etching.
【0018】[0018]
【表1】 [Table 1]
【0019】表1の如くγFe2O3と炭素系被膜は、通
常界面にC−Oボンディングを形成する為、密着性が極
端に低下することがあり、磁気ディスク等の保護膜とし
て応用する場合大きな問題となっている。As shown in Table 1, since γFe 2 O 3 and a carbon-based film usually form a CO bond at the interface, the adhesiveness may be extremely reduced, and when applied as a protective film for a magnetic disk or the like. It is a big problem.
【0020】そこで、表1に示すような比較をおこなっ
た結果基本的にはO2を使わないプロセスが良いと思わ
れるが、例え使ってもH2でプラズマ処理して置換する
工程を取り入れれば、密着性は大きく改善されることが
判明した。Siウエハの場合は界面の化学結合がSi−
Cとなる為、大きな差は出ないがSi表面に酸素原子、
分子、ラジカル等が吸着していると密着性を低下させる
原因となる。Therefore, as a result of comparison as shown in Table 1, it is considered that a process not using O 2 is basically good. However, even if it is used, a process of performing a plasma treatment with H 2 for replacement is adopted. For example, it was found that the adhesion was greatly improved. In the case of a Si wafer, the chemical bond at the interface is Si-
C, so there is no big difference, but oxygen atoms,
When molecules, radicals, and the like are adsorbed, they cause a decrease in adhesion.
【0021】H2プラズマエッチングは、エッチング速
度が極端に遅いのでスループットを上げ、量産性を考え
れば、O2プラズマエッチングとH2プラズマクリーニン
グの併用による方法が現時点では良好と考える。Since the etching rate of the H 2 plasma etching is extremely low, the throughput is increased, and from the viewpoint of mass productivity, it is considered that a method using both the O 2 plasma etching and the H 2 plasma cleaning is good at present.
【0022】[0022]
【発明の効果】本発明によれば、炭素または炭素を主成
分とする被膜を除去した後に、クリーニング用気体例え
ばAr、H2を用い、反応室内を清浄化することが可能
になった。また、上記方法にて、清浄化後通常の膜を形
成すると、密着性に大きな改善がみられた。According to the present invention, the reaction chamber can be cleaned using a cleaning gas such as Ar or H 2 after removing carbon or a film containing carbon as a main component. In addition, when a normal film was formed after cleaning by the above method, a great improvement in adhesion was observed.
【0023】このことから、磁気記録媒体である磁気テ
ーブ、磁気ディスク等のファイナルパシベーション膜に
用いることが始めて可能となった。また、半導体集積回
路等のファイナルコーティングの絶縁膜に用いることが
可能となった。For this reason, it has become possible for the first time to use it for a final passivation film of a magnetic recording medium such as a magnetic tape or a magnetic disk. Further, it can be used as an insulating film of a final coating such as a semiconductor integrated circuit.
【図1】各エッチング気体におけるエッチング速度及び
セルフバイアスを示した図。FIG. 1 is a diagram showing an etching rate and a self-bias in each etching gas.
【図2】本発明に使用したプラズマ装置の概略図を示す
図。FIG. 2 is a diagram showing a schematic view of a plasma apparatus used in the present invention.
【図3】実施例で用いた基板と基板上に形成された炭素
系被膜を示す図。FIG. 3 is a view showing a substrate used in an example and a carbon-based film formed on the substrate.
Claims (7)
炭素を主成分とする被膜を形成する方法であって、 酸素のプラズマを発生させて前記反応室内の不要部分に
付着した炭素または炭素を主成分とする膜を除去し、前
記反応室内に前記磁気記録媒体を搬入し、前記磁気記録
媒体上に前記炭素または炭素を主成分とする被膜を形成
することを特徴とする炭素または炭素を主成分とする被
膜の形成方法。1. A method for forming a coating containing carbon or carbon as a main component on a magnetic recording medium in a reaction chamber, comprising generating oxygen plasma to remove carbon or carbon attached to unnecessary portions in the reaction chamber. Removing the film containing the main component, loading the magnetic recording medium into the reaction chamber, and forming the coating containing the carbon or carbon as the main component on the magnetic recording medium. A method for forming a coating as a component.
炭素を主成分とする被膜を形成する方法であって、 弗化物気体のプラズマを発生させて前記反応室内の不要
部分に付着した炭素または炭素を主成分とする膜を除去
し、前記反応室内に前記磁気記録媒体を搬入し、前記磁
気記録媒体上に前記炭素または炭素を主成分とする被膜
を形成することを特徴とする炭素または炭素を主成分と
する被膜の形成方法。2. A method for forming a coating containing carbon or carbon as a main component on a magnetic recording medium in a reaction chamber, comprising generating plasma of a fluoride gas to remove carbon or carbon adhering to an unnecessary portion in the reaction chamber. Removing the film containing carbon as a main component, carrying the magnetic recording medium into the reaction chamber, and forming a film containing carbon or carbon as a main component on the magnetic recording medium. A method for forming a coating mainly composed of
たは炭素を主成分とする被膜を形成する方法であって、 酸素のプラズマを発生させて前記反応室内の不要部分に
付着した炭素または炭素を主成分とする膜を除去し、前
記反応室内に前記半導体集積回路を搬入し、前記半導体
集積回路上に前記炭素または炭素を主成分とする被膜を
形成することを特徴とする炭素または炭素を主成分とす
る被膜の形成方法。3. A method for forming a carbon or carbon-based coating film on a semiconductor integrated circuit body in a reaction chamber, the method comprising generating oxygen plasma and depositing carbon or carbon adhered to an unnecessary portion in the reaction chamber. Removing the film containing carbon as a main component, carrying the semiconductor integrated circuit into the reaction chamber, and forming a film containing carbon or carbon as a main component on the semiconductor integrated circuit. A method for forming a coating as a main component.
たは炭素を主成分とする被膜を形成する方法であって、 弗化物気体のプラズマを発生させて前記反応室内の不要
部分に付着した炭素または炭素を主成分とする膜を除去
し、前記反応室内に前記半導体集積回路を搬入し、前記
半導体集積回路上に前記炭素または炭素を主成分とする
被膜を形成することを特徴とする炭素または炭素を主成
分とする被膜の形成方法。4. A method for forming a film containing carbon or carbon as a main component on a semiconductor integrated circuit body in a reaction chamber, the method comprising generating plasma of a fluoride gas to remove carbon adhering to an unnecessary portion in the reaction chamber. Or removing the film containing carbon as a main component, carrying the semiconductor integrated circuit into the reaction chamber, and forming the film containing carbon or carbon as a main component on the semiconductor integrated circuit. A method for forming a coating mainly composed of carbon.
炭化水素気体のプラズマを発生させることによって前記
炭素または炭素を主成分とする被膜を形成することを特
徴とする炭素または炭素を主成分とする被膜の形成方
法。5. The method according to claim 1, wherein:
A method for forming a carbon- or carbon-based coating film, comprising forming the carbon- or carbon-based coating film by generating a hydrocarbon gas plasma.
炭化水素気体に高周波エネルギーを加えてプラズマを発
生させることによって前記炭素または炭素を主成分とす
る被膜を形成することを特徴とする炭素または炭素を主
成分とする被膜の形成方法。6. The method according to claim 1, wherein:
A method for forming a carbon- or carbon-based coating, characterized by forming the carbon- or carbon-based coating by generating plasma by applying high-frequency energy to a hydrocarbon gas.
2.45GHzのマイクロ波によって前記炭化水素気体に
エネルギーを加えてプラズマを発生させることによって
前記炭素または炭素を主成分とする被膜を形成すること
を特徴とする炭素または炭素を主成分とする被膜の形成
方法。ることを特徴とする炭素または炭素を主成分とす
る被膜の形成方法。7. The method according to claim 1, wherein:
2. A method of forming a carbon or carbon-based film by applying energy to the hydrocarbon gas by microwaves of 2.45 GHz to generate plasma. Forming method. Forming a film containing carbon or carbon as a main component.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP36989899A JP3256209B2 (en) | 1988-08-11 | 1999-12-27 | Method of forming carbon or carbon-based coating |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP36989899A JP3256209B2 (en) | 1988-08-11 | 1999-12-27 | Method of forming carbon or carbon-based coating |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP20253488A Division JP3180332B2 (en) | 1988-08-11 | 1988-08-11 | Method of cleaning apparatus for forming carbon or carbon-based coating |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2000199065A true JP2000199065A (en) | 2000-07-18 |
JP3256209B2 JP3256209B2 (en) | 2002-02-12 |
Family
ID=18495589
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP36989899A Expired - Lifetime JP3256209B2 (en) | 1988-08-11 | 1999-12-27 | Method of forming carbon or carbon-based coating |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP3256209B2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7192874B2 (en) | 2003-07-15 | 2007-03-20 | International Business Machines Corporation | Method for reducing foreign material concentrations in etch chambers |
-
1999
- 1999-12-27 JP JP36989899A patent/JP3256209B2/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7192874B2 (en) | 2003-07-15 | 2007-03-20 | International Business Machines Corporation | Method for reducing foreign material concentrations in etch chambers |
US7517802B2 (en) | 2003-07-15 | 2009-04-14 | International Business Machines Corporation | Method for reducing foreign material concentrations in etch chambers |
Also Published As
Publication number | Publication date |
---|---|
JP3256209B2 (en) | 2002-02-12 |
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