JPH02217471A - Manufacture of carbon-based film - Google Patents
Manufacture of carbon-based filmInfo
- Publication number
- JPH02217471A JPH02217471A JP1036897A JP3689789A JPH02217471A JP H02217471 A JPH02217471 A JP H02217471A JP 1036897 A JP1036897 A JP 1036897A JP 3689789 A JP3689789 A JP 3689789A JP H02217471 A JPH02217471 A JP H02217471A
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- film
- stress
- gas
- based film
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 22
- 229910052799 carbon Inorganic materials 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 239000007789 gas Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 14
- -1 composed of carbon Chemical compound 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 3
- 239000012808 vapor phase Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 description 37
- 230000035882 stress Effects 0.000 description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 230000008646 thermal stress Effects 0.000 description 7
- 238000000576 coating method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000002040 relaxant effect Effects 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- OOBJYKUGPRVRSK-UHFFFAOYSA-N azane;trihydrofluoride Chemical compound N.F.F.F OOBJYKUGPRVRSK-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
「発明の利用分野」
本発明は、炭素または炭素を主成分とする被膜（以下炭
素系被膜という）を応用する上で、下地基材に対し界面
特性、特に密着性を向上させ、炭素系被膜の特徴である
耐摩擦性、高平滑性、高硬度等の緒特性を最大限に引き
出すものである。Detailed Description of the Invention "Field of Application of the Invention" The present invention relates to the application of carbon or a film containing carbon as a main component (hereinafter referred to as a carbon-based film) to the underlying base material, and to improve the interfacial properties, particularly the adhesion. This improves the properties of carbon-based coatings, and maximizes the characteristics of carbon-based coatings such as friction resistance, high smoothness, and high hardness.
「従来の技術」
従来より、多種多様な基材に炭素系被膜を形成すること
が試みられているが、界面におけるさまざまな要因、例
えば格子定数の不整から生ずる界面応力、熱膨張係数の
違いによる成膜後の収縮率の差より生ずる熱応力などに
より、必ずしも満足のいく密着性が得られていないのが
現状である。``Prior art'' Previously, attempts have been made to form carbon-based films on a wide variety of base materials. At present, it is not always possible to obtain satisfactory adhesion due to thermal stress caused by differences in shrinkage rates after film formation.
「従来技術の問題点」
炭素系被膜は、高硬度という長所を持ちながら反面、大
きな残留応力を保有している為、下地基板依存性、並び
に膜厚依存性という特殊な物性を備えている。``Problems with conventional technology'' Carbon-based coatings have the advantage of high hardness, but on the other hand, they also have large residual stress, so they have special physical properties such as dependence on the underlying substrate and dependence on film thickness.
すなわち、膜厚とともに全応力（膜厚方向に積分した応
力）が高くなるが、炭素系被膜のもつ応力を下地基材自
身で緩和できるものがあり、また炭素系被膜自身の残留
応力は膜厚限界という定義で、耐えられる膜厚が決定さ
れ、所望の膜厚が得られないという現状があり、新しい
技術の開発が急がれている。In other words, the total stress (stress integrated in the film thickness direction) increases with film thickness, but the stress of some carbon-based films can be alleviated by the underlying substrate itself, and the residual stress of the carbon-based film itself increases as the film thickness increases. The current situation is that the film thickness that can withstand is determined by the definition of a limit, and the desired film thickness cannot be obtained, so there is an urgent need to develop new technologies.
本発明は以上のような残留応力を低下させることを目的
としてなされたものである。The present invention has been made for the purpose of reducing the above-mentioned residual stress.
ｒ問題を解決すべき手段」
そのため本発明は炭素系被膜を形成する化学的気相法に
おいて、出発原料気体に水素化合物を用いる際に、添加
気体として、Ｎ２、ＮＦ３を加えることを特徴とする炭
素系被膜の作製方法としたものである。Therefore, the present invention is characterized in that when a hydrogen compound is used as a starting material gas in a chemical vapor phase method for forming a carbon-based film, N2 and NF3 are added as additive gases. This is a method for producing a carbon-based film.
本発明は、炭素系被膜の内部応力が膜中の水素含有量に
依存することに着目し、公知の化学的気相法において水
素化合物、例えばＣＨ，、ＣｆＨ，。The present invention focuses on the fact that the internal stress of a carbon-based film depends on the hydrogen content in the film, and uses a hydrogen compound such as CH, CfH, etc. in a known chemical vapor phase method.
ＣｆＨ，等を出発原料気体に使用し、水素を添加するの
ではなく、Ｎ、、ＮＦ、等を添加し、膜中のＣ−１（結
合のＨをＮと置換させることによって、内部応力を初期
及び経時において制御することを可能としたものである
。CfH, etc. are used as the starting material gas, and instead of adding hydrogen, N, NF, etc. are added, and the internal stress is reduced by replacing H in the C-1 (bond) in the film with N. This allows for control both initially and over time.
炭素被膜の基本的なコーティングに関しては、本出願人
の出願になる特許願「炭素または炭素を主成分とする被
膜を形成する方法」 （昭和６３年３月２日出１１）」
が知られている。Regarding the basic coating of carbon film, please refer to the patent application filed by the present applicant entitled "Method of forming carbon or a film containing carbon as a main component" (March 2, 1988, issue 11).
It has been known.
以下実施例に従って本発明を説明する。The present invention will be explained below according to Examples.
「実施例」
第１図は平行平板型プラズマ装置でガス系（１）におい
て、まず反応性気体である炭化水素気体を（２）より添
加気体である窒素、沸化窒素を（３）より、またこれら
の被膜のエツチング気体として酸素を（４）より、クリ
ーニング用として水素、アルゴルを（５）より、流量針
（６）、バルブ（７）を介してノズル（８）より、反応
系（９）の中に導入する。``Example'' Figure 1 shows a parallel plate plasma device in which in the gas system (1), a reactive gas, hydrocarbon gas, is first added to (2), and nitrogen and fluoride nitrogen are added to the gas system (3). In addition, oxygen is supplied as an etching gas for these films from (4), hydrogen and Algol are supplied for cleaning from (5), and a reaction system (9) is supplied from a nozzle (8) via a flow rate needle (6) and a valve (7). ).
反応性気体は、メタン（ＣＩ＋４）、エタン（ｃｚｕｈ
）、エチレンＣＣ＊Ｈａ ） 、メタン系炭化水素（Ｃ
ｆｉＨｚ−ｚ）等の気体または珪素を一部に含んだ場合
はテトラメチルシラン（（Ｃ１ｌｓ）４ｓｉ）、テトラ
エラルシラン（（ＣＪｓ） ｎ５ｉ）のような炭化珪素
であっても、また四塩化炭素（ＣＣＩ ｍ ）のような
塩化炭素であってもよい。Reactive gases include methane (CI+4), ethane (czuh
), ethylene CC*Ha ), methane hydrocarbons (C
silicon carbide such as tetramethylsilane ((C1ls)4si), tetraeralsilane ((CJs) n5i), or carbon tetrachloride. It may also be carbon chloride such as (CCI m ).
反応系（９）では、減圧下にて炭素系被膜の成膜および
、それらのエツチング処理等を行う。反応系（９）内は
、第１の電極０１）、第２の電極Ｑ２）を有し、被膜形
成基材００は、第２の電極０２）すなわち高周波電力給
電側に設置される。一対の電極（１１）（１２）間には
、高周波電源（ロ）マツチングトランス０５）、直流バ
イア１電源Ｏｅより高周波電気エネルギーが加えられ、
プラズマＱ３１が発生する。その結果、特定の成膜条件
において、所望の炭素系被膜が得られる。In the reaction system (9), a carbon-based film is formed and etched thereon under reduced pressure. The inside of the reaction system (9) has a first electrode 01) and a second electrode Q2), and the film-forming substrate 00 is installed on the second electrode 02), that is, on the high-frequency power feeding side. High frequency electrical energy is applied between the pair of electrodes (11) and (12) from a high frequency power source (b) matching transformer 05) and a DC via 1 power source Oe.
Plasma Q31 is generated. As a result, a desired carbon-based coating can be obtained under specific film-forming conditions.
反応後の不要物は排気系の圧力調整バルブ０７）ターボ
分子ポンプ側、ロータリーポンプ（９）を経て排気され
る。Unwanted substances after the reaction are exhausted through the pressure regulating valve 07 of the exhaust system, the turbomolecular pump side, and the rotary pump (9).
本実施例において、成膜条件は、反応温度ＲＴ〜３５０
°Ｃ反応圧力０．０１〜０．５ｔｏｒｒ高周波電力密度
０．１〜０．３Ｗ／ｃｄセルフバイアス電圧−１５０Ｖ
〜−２５０Ｖであり、原料気体であるＣｚＨａ、Ｎｚ
はｃ、Ｈ，／ Ｎｚ比を０．０５〜０．５の範囲で可変
し、膜のトータルの残留応力を決定している熱応力及び
膜中水素台を量をコントロールしている。In this example, the film forming conditions were as follows: reaction temperature RT~350
°C reaction pressure 0.01~0.5torr high frequency power density 0.1~0.3W/cd self bias voltage -150V
~-250V, and the raw material gas CzHa, Nz
The c, H,/Nz ratio is varied in the range of 0.05 to 0.5 to control the amount of thermal stress and hydrogen content in the film, which determine the total residual stress of the film.
第２図は、形成した膜の全応力を基板温度を可変して検
討したものであり、一般のＣＶＤにより形成される薄膜
と同様に基板温度の上昇と共に熱応力が相対的に増加す
る為、全応力は増える傾向を示している。この場合の基
本的な条件は反応圧力を０．０３７５ｔｏｒｒ、高周波
電力密度を０．１５Ｗ／ｃｄ、セルフバイアス電圧が一
２１０■においてＣ２Ｈ４／Ｎ！比−〇、５であった。Figure 2 shows a study of the total stress of the formed film by varying the substrate temperature.As with thin films formed by general CVD, the thermal stress relatively increases as the substrate temperature rises. The total stress shows a tendency to increase. The basic conditions in this case are reaction pressure of 0.0375 torr, high frequency power density of 0.15 W/cd, self-bias voltage of 1210 cm, and C2H4/N! The ratio was -〇, 5.
第３図は熱応力を含めた圧縮応力をＣ，Ｌ／ Ｎ２比を
可変させて調べたもので添加ガスであるＮ２を増やすこ
とによって、膜中のＣ−Ｈ結合は、Ｎ−Ｈ結合の形で置
換され、相対的に膜中の水素含有量は減少する。すなわ
ち、構造緩和効果が低下し、大きな残留応力という形で
とり残されるものである。Figure 3 shows the results of examining the compressive stress including thermal stress by varying the C, L/N2 ratio. By increasing the added gas N2, the C-H bonds in the film are changed to the N-H bonds. The hydrogen content in the film is relatively reduced. In other words, the structural relaxation effect is reduced and a large residual stress is left behind.
第４図は、赤外吸収スペクトルの２９６０〜２８５０ｃ
ｍ１付近のｓｐ”結合による吸収量から概算した膜中水
素含有量と圧縮応力の関係を示したものであるが、膜中
水素含有量は炭化水素気体に、水素を添加した方が低減
されるが、膜内部構造の歪を増大し、残留応力として残
ってしまい好ましいものでなく、また、Ｎ２、ＮＦ、等
を添加すると膜中のＣ−Ｈ結合のＨをＮと置換させるこ
とが可能で、残留応力を生じさせずに大きな原子間結合
エネルギーにより非晶質ではあるが、内部構造緩和効果
を合わせもち、熱応力とＣ−Ｈ結合の相互関係を抑制し
、内部応力を制御することができる。Figure 4 shows the infrared absorption spectrum from 2960 to 2850c.
This figure shows the relationship between the hydrogen content in the film and the compressive stress, estimated from the absorption amount by the sp" bond near m1, and the hydrogen content in the film is reduced by adding hydrogen to the hydrocarbon gas. However, this is not desirable as it increases the strain in the internal structure of the film and remains as residual stress.Additionally, adding N2, NF, etc. can replace H in the C-H bonds in the film with N. Although it is amorphous due to large interatomic bond energy without producing residual stress, it also has the effect of relaxing the internal structure, suppressing the interaction between thermal stress and C-H bonds, and controlling internal stress. can.
すなわち、膜中水素含有量の制御として、熱応力と内部
応力とからなる残留応力を基板温度とＣ−Ｈ結合／Ｃ−
Ｎ結合比等の相関関係により、コントロール可能である
ことを示している。In other words, to control the hydrogen content in the film, the residual stress consisting of thermal stress and internal stress is controlled by changing the substrate temperature and C-H bond/C-
This shows that it can be controlled by correlations such as N-bond ratio.
「効果」
本発明によれば、従来むずかしいとされていた炭素系被
膜の応用に際し、熱応力と内部応力とからなる残留応力
を単に膜中水素含有量の低減だけでなく、さらに別の元
素、例えば窒素との置換という形で構成することで、内
部構造緩和効果をもたらし、界面との密着性、耐熱性の
初期ならびに経時変化に対し、多大な改善効果がある。"Effect" According to the present invention, when applying a carbon-based film, which has been considered difficult in the past, residual stress consisting of thermal stress and internal stress can be reduced not only by reducing the hydrogen content in the film, but also by adding another element, For example, by replacing it with nitrogen, it brings about an effect of relaxing the internal structure, and has a great effect of improving the adhesion with the interface and the initial and aging changes in heat resistance.
以上により、同時に下地基材との界面に生ずる。As a result of the above, it simultaneously occurs at the interface with the underlying base material.
界面応力も低減することに成功し、初めて工業的に実用
可能となったものである。It also succeeded in reducing interfacial stress, making it commercially viable for the first time.
第１図は本発明の実施に使用した平行平板プラズマ装置
の概要を示す。
第２図は成膜時の基板温度と全応力の関係を示す図。
第３図は成膜時のＣｔＨａｌＮｚ比と圧縮応力の関係を
示す図。
第４図は高抵抗シリコンウェハー上に形成した被膜の膜
中水素含有量と圧縮応力の関係を示す図。FIG. 1 shows an outline of a parallel plate plasma apparatus used to carry out the present invention. FIG. 2 is a diagram showing the relationship between substrate temperature and total stress during film formation. FIG. 3 is a diagram showing the relationship between CtHalNz ratio and compressive stress during film formation. FIG. 4 is a diagram showing the relationship between hydrogen content in a film formed on a high-resistance silicon wafer and compressive stress.
Claims (1)
的気相法において、出発原料気体に水素化合物を用いる
際に、添加気体として、Ｎ＿２、ＮＦ＿３を加えること
を特徴とする炭素系被膜の作製方法。 ２、特許請求の範囲第１項に記載の添加気体は原料気体
に対して５〜５０％の範囲であることを特徴とする。[Claims] 1. In the chemical vapor phase method for forming carbon or a film mainly composed of carbon, when a hydrogen compound is used as the starting material gas, N_2 and NF_3 are added as additive gases. A method for producing a carbon-based film. 2. The added gas according to claim 1 is characterized in that the amount of the added gas is in the range of 5 to 50% based on the raw material gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1036897A JP2775278B2 (en) | 1989-02-16 | 1989-02-16 | Preparation method of carbon-based coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1036897A JP2775278B2 (en) | 1989-02-16 | 1989-02-16 | Preparation method of carbon-based coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02217471A true JPH02217471A (en) | 1990-08-30 |
| JP2775278B2 JP2775278B2 (en) | 1998-07-16 |
Family
ID=12482568
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1036897A Expired - Lifetime JP2775278B2 (en) | 1989-02-16 | 1989-02-16 | Preparation method of carbon-based coating |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2775278B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03274269A (en) * | 1990-03-22 | 1991-12-05 | Matsushita Electric Ind Co Ltd | Method for synthesizing diamondlike thin film and diamondlike thin film |
| US5296258A (en) * | 1992-09-30 | 1994-03-22 | Northern Telecom Limited | Method of forming silicon carbide |
| US5515201A (en) * | 1992-08-28 | 1996-05-07 | Lunax Company Limited | Microscope-telescope combination fitted with illuminating apparatus |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63210010A (en) * | 1987-02-24 | 1988-08-31 | Semiconductor Energy Lab Co Ltd | Production of carbon |
| JPS6475678A (en) * | 1987-09-17 | 1989-03-22 | Sumitomo Electric Industries | Hard carbon film containing nitrogen |
-
1989
- 1989-02-16 JP JP1036897A patent/JP2775278B2/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63210010A (en) * | 1987-02-24 | 1988-08-31 | Semiconductor Energy Lab Co Ltd | Production of carbon |
| JPS6475678A (en) * | 1987-09-17 | 1989-03-22 | Sumitomo Electric Industries | Hard carbon film containing nitrogen |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03274269A (en) * | 1990-03-22 | 1991-12-05 | Matsushita Electric Ind Co Ltd | Method for synthesizing diamondlike thin film and diamondlike thin film |
| US5515201A (en) * | 1992-08-28 | 1996-05-07 | Lunax Company Limited | Microscope-telescope combination fitted with illuminating apparatus |
| US5296258A (en) * | 1992-09-30 | 1994-03-22 | Northern Telecom Limited | Method of forming silicon carbide |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2775278B2 (en) | 1998-07-16 |
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