JP2009270202A - Surface treatment method and vacuum vessels - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004381 surface treatment Methods 0.000 title claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- 239000000758 substrate Substances 0.000 claims 1
- 150000002431 hydrogen Chemical class 0.000 abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000009489 vacuum treatment Methods 0.000 abstract 1
- ADKPKEZZYOUGBZ-UHFFFAOYSA-N [C].[O].[Si] Chemical compound [C].[O].[Si] ADKPKEZZYOUGBZ-UHFFFAOYSA-N 0.000 description 10
- 239000002131 composite material Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910001868 water Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000010943 off-gassing Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910018540 Si C Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- NDOBYZHQZWIIDH-UHFFFAOYSA-N [C].[N].[O].[Si] Chemical compound [C].[N].[O].[Si] NDOBYZHQZWIIDH-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- -1 siloxanes Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- DZPJVKXUWVWEAD-UHFFFAOYSA-N [C].[N].[Si] Chemical compound [C].[N].[Si] DZPJVKXUWVWEAD-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- ZSMNRKGGHXLZEC-UHFFFAOYSA-N n,n-bis(trimethylsilyl)methanamine Chemical compound C[Si](C)(C)N(C)[Si](C)(C)C ZSMNRKGGHXLZEC-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明は、真空装置の真空容器や真空容器内部品等の真空容器類の表面にガス放出の少ない均質な膜を堆積させる表面処理方法及び真空容器類に関するものである。 The present invention relates to a surface treatment method and a vacuum container for depositing a homogeneous film with little gas release on the surface of a vacuum container such as a vacuum container of a vacuum apparatus or a component in the vacuum container.
従来、真空容器の排気において、容器の圧力降下速度を速くする目的として、真空容器内壁及び真空容器内部品の表面からガスの放出速度を少なくするために窒化チタンやシリコン（特許文献１参照）を成膜することが行われていた。これら膜の成膜においては、原料にチタン、シリコン等の固体を用いるいことが多かった。また、電子産業でアモルファスシリコンを成膜するためにシラン等の気体を原料にした平行平板のＣＶＤが行われている。 Conventionally, in evacuation of a vacuum vessel, titanium nitride or silicon (see Patent Document 1) is used to reduce the gas release rate from the surface of the inner wall of the vacuum vessel and the parts in the vacuum vessel in order to increase the pressure drop rate of the vessel. Film formation was performed. In forming these films, it is often desirable to use a solid such as titanium or silicon as a raw material. In addition, parallel plate CVD using a gas such as silane as a raw material is performed in the electronics industry to form amorphous silicon.
しかしながら、ガス放出を少なくするためには、真空容器や容器内部品の全面をガス放出の少ない膜で被覆しなければならないが、一般的に真空容器や真空容器内部品の形状は複雑であり、固体を原料にする前者の方法では、ガス放出の少ない均質な膜を全面に成膜することは技術的に困難であった。また、シラン等の気体を原料にした平行平板のＣＶＤによる後者の方法では、３次元構造物の真空容器内壁に成膜することはできないという問題点があった。
この発明は上記のような従来技術の問題点を解決するもので、真空装置の真空容器内壁や真空容器内部品等の真空容器類の表面全面にガス放出の少ない均質な膜を成膜する表面処理方法及び真空容器類を提供することを目的としている。
However, in order to reduce gas emission, the entire surface of the vacuum vessel and the components in the vessel must be covered with a film with a low gas emission, but generally the shape of the vacuum vessel and the components in the vacuum vessel is complicated, In the former method using a solid as a raw material, it has been technically difficult to form a homogeneous film with little outgassing on the entire surface. Further, the latter method using parallel plate CVD using a gas such as silane as a raw material has a problem in that a film cannot be formed on the inner wall of a vacuum vessel of a three-dimensional structure.
The present invention solves the above-mentioned problems of the prior art, and is a surface on which a uniform film with little outgassing is formed on the entire surface of the vacuum vessel such as the inner wall of the vacuum vessel and the parts inside the vacuum vessel. It aims at providing a processing method and vacuum containers.
本発明の表面処理方法は、前記目的を達成するべく、請求項１記載の通り、窒素及び酸素のうち少なくとも１種類の元素と、水素と、炭素とが含まれたシリコン化合物を原料とし、この原料を１０−３〜１０−５Ｐａの圧力に減圧された処理容器に気体状態で導入し、該原料によるプラズマを生成することにより、シリコン、水素と炭素及び酸素、窒素の少なくとも１種類の元素が含まれた膜を、この減圧された処理容器内に収容した被処理真空容器類の表面に堆積させることを特徴とする。
また、請求項２記載の表面処理方法は、請求項１記載の表面処理方法において、前記シリコン化合物を２種類以上とすることを特徴とする。
また、請求項３記載の表面処理方法は、請求項１または２の何れかに記載の表面処理方法において、前記容器内にヘリウム、アルゴンガス等の不活性ガスを導入させてクリーニング処理をしてから、前記膜の堆積を行うことを特徴とする。
また、請求項４記載の表面処理方法は、請求項１乃至３の何れかに記載の表面処理方法において、前記堆積された膜を、大気中で、或いは、真空中で１００〜５００℃の温度で加熱することを特徴とする。
また、本発明の真空容器類は、請求項５記載の通り、請求項１乃至４の何れかに記載の方法により表面処理されたことを特徴とする。
In order to achieve the object, the surface treatment method of the present invention uses, as a raw material, a silicon compound containing at least one element of nitrogen and oxygen, hydrogen, and carbon, as described in
The surface treatment method according to
The surface treatment method according to
The surface treatment method according to
Moreover, the vacuum containers of the present invention are characterized in that, as described in
以上説明した通り、本発明によれば、水素と炭素と、窒素、酸素のうち少なくとも１種類の元素が含まれた気体状のシリコン化合物を放電させることで分解し、シリコン−酸素−炭素、シリコン−窒素−炭素、或いは、シリコン−酸素−窒素−炭素の複合膜を成膜するので、真空容器の表面及び部品表面の全面にガス放出の少ない均質な膜を形成することができ、真空排気の際に目的とする真空状態に到達するまでの排気時間を短縮することができる。かくして、ガス放出の少ない均質な膜を備えた真空容器類が得られる。
これを詳述すれば、カーボンやシリコンやゲルマニウムなどのＩＶ属の材料は水の初期付着確率が低く、また、シリコンやゲルマニウムの材料は大気中の水及び酸素により自然に酸化されて表面が安定な酸化物、或いは、水酸化物になる。こうしてできた酸化物や水酸化物は不活性であり通常真空容器の材料として用いられるステンレス鋼やアルミニウム合金などよりも水が吸着しにくいという性質がある。また、これらの性質は、膜中に水素、酸素、窒素などの非金属元素が含まれていても変化しない。被膜として、Ｓｉ−Ｃ−Ｏ、Ｓｉ−Ｃ−Ｎを用いた場合でもこれらの表面は自然に酸化されて、これらの酸化被膜が形成されることになる。かかる酸化物からなる被膜で覆われた容器の内壁には水が吸着しにくくなるので真空排気の際に容器内の水が排出されやすくなり目的とする真空状態に到達するまでの排気時間を短縮することができる。
As described above, according to the present invention, the silicon-oxygen-carbon, silicon is decomposed by discharging a gaseous silicon compound containing at least one element of hydrogen, carbon, nitrogen, and oxygen. -Since a composite film of nitrogen-carbon or silicon-oxygen-nitrogen-carbon is formed, a homogeneous film with little outgassing can be formed on the entire surface of the vacuum vessel and the part surface. In this case, it is possible to shorten the exhaust time until the target vacuum state is reached. Thus, vacuum containers having a homogeneous film with little outgassing can be obtained.
To elaborate, Group IV materials such as carbon, silicon, and germanium have a low initial sticking probability of water, and silicon and germanium materials are naturally oxidized by water and oxygen in the atmosphere to stabilize the surface. Oxide or hydroxide. The oxides and hydroxides thus formed are inert and have the property that water is less likely to adsorb than stainless steel and aluminum alloys that are usually used as materials for vacuum containers. These properties do not change even if the film contains non-metallic elements such as hydrogen, oxygen, and nitrogen. Even when Si—C—O or Si—C—N is used as the coating, these surfaces are naturally oxidized to form these oxide coatings. The inner wall of the container covered with such an oxide film is less likely to adsorb water, so that the water in the container is easily discharged during vacuum evacuation, shortening the exhaust time until the target vacuum state is reached. can do.
本発明の表面処理方法に用いる原料である、水素と炭素と、窒素、酸素のうち少なくとも１種類の元素が含まれたシリコン化合物としては、テトラメチルジシロキサン、ヘキサメチルジシロキサン等のシロキサン、テトラメトキシシラン、テトラエトキシシラン等のアルコキシシラン、ヘプタメチルジシラザン、ヘキサメチルジシラザン等のシラザが挙げられる。これら原料シリコン化合物は、１種類のみ用いても、２種以上を用いるようにしてもよい。
即ち、シリコン−酸素−炭素、シリコン−窒素−炭素、或いは、シリコン−酸素−窒素−炭素の複合膜を成膜できれば、いかなるシリコン化合物でも使用できる。
Examples of a silicon compound containing at least one element among hydrogen, carbon, nitrogen, and oxygen, which are raw materials used in the surface treatment method of the present invention, include siloxanes such as tetramethyldisiloxane and hexamethyldisiloxane, tetra Examples include alkoxysilanes such as methoxysilane and tetraethoxysilane, and silazanes such as heptamethyldisilazane and hexamethyldisilazane. These raw material silicon compounds may be used alone or in combination of two or more.
That is, any silicon compound can be used as long as a silicon-oxygen-carbon, silicon-nitrogen-carbon, or silicon-oxygen-nitrogen-carbon composite film can be formed.
前記処理容器内は、１０-3〜１０-5Ｐａ程度の圧力に減圧し、この減圧された処理容器に前記原料を気体状態で導入し、該原料によるプラズマを生成することにより、シリコン、水素と炭素及び酸素、窒素の少なくとも１種類の元素が含まれた膜を、この減圧された処理容器内に収容した被処理真空容器類の表面に堆積させるわけであるが、この処理容器内に被処理真空容器や被処理真空容器内部品等の被処理真空容器類を収容する。 The inside of the processing vessel is depressurized to a pressure of about 10 −3 to 10 −5 Pa, the raw material is introduced into the reduced pressure processing vessel in a gaseous state, and plasma is generated from the raw material, thereby generating silicon, hydrogen, And a film containing at least one element of carbon, oxygen, and nitrogen is deposited on the surface of the vacuum containers to be processed accommodated in the decompressed processing container. Houses vacuum containers to be processed such as processing vacuum containers and parts in vacuum containers to be processed.
前記処理容器内に、ヘリウム、アルゴンガス等の不活性ガスを導入させてクリーニング処理を行ってから、前記膜の堆積を行うようにすれば、より、良好な成膜を行うことができる。 If the film is deposited after introducing an inert gas such as helium or argon gas into the processing container and performing the cleaning process, better film formation can be performed.
前記処理容器内の温度は、室温〜５００℃程度に設定して、前記膜の堆積を行うようにすればよい。これは、ポラースでない緻密な膜を形成できるからである。 The temperature in the processing vessel may be set to room temperature to about 500 ° C. to deposit the film. This is because a dense film that is not porous can be formed.
また、前記堆積された膜を、大気中、或いは、１００〜５００℃の温度で加熱することで、膜中に取り込まれた余分な気体や表面に吸着した余分な水分を除去することができるので、このような加熱処理を行うことが好ましい。 Further, by heating the deposited film in the atmosphere or at a temperature of 100 to 500 ° C., excess gas taken in the film and excess moisture adsorbed on the surface can be removed. It is preferable to perform such heat treatment.
前記表面処理方法の対象となる真空容器類には、真空装置の真空容器や真空容器内部品等が含まれる。 The vacuum containers to be subjected to the surface treatment method include a vacuum container of a vacuum apparatus, parts in the vacuum container, and the like.
以下、本発明の実施例を図面に基づいて説明する。
図１は成膜を行うための（真空）処理容器の中に、表面処理を行う真空容器を入れて表面処理を実施した例である。
図１において、１は表面にシリコン化合物の成膜をされる被処理真空容器、２は電流導入端子、３は直流電源、４は原料のシリコン化合物、５はマスフローコントローラー、６は圧力計、７は成膜を行うための処理容器、８は可変コンダクタンスバルブである。
Embodiments of the present invention will be described below with reference to the drawings.
FIG. 1 shows an example in which a surface treatment is performed by placing a vacuum vessel for surface treatment in a (vacuum) treatment vessel for film formation.
In FIG. 1, 1 is a vacuum container to be processed on which a silicon compound is formed, 2 is a current introduction terminal, 3 is a DC power source, 4 is a raw material silicon compound, 5 is a mass flow controller, 6 is a pressure gauge, 7 Is a processing container for forming a film, and 8 is a variable conductance valve.
本実施例では、表面にシリコン化合物の成膜をされる被処理真空容器１として、ステンレス鋼で作製し内面を電解研磨処理したものを用いた。この被処理真空容器１を（真空）処理容器７に入れ、（真空）処理容器７を１０-4Ｐａ程度に排気した。
In this example, the
本実施例では原料シリコン化合物４として、ヘキサメチルジシロキサンを用い、この原料ヘキサメチルジシロキサン４をマスフローコントローラー５を通して、（真空）処理容器７内に導入し、バルブ８を用いて圧力計６の圧力が１０Ｐａになるように調整しながら、直流電源３に１ｋＶの電圧を印加しグロー放電によりプラズマを発生させ、被処理真空容器１の全面にシリコン−酸素−炭素の複合膜を成膜した。
In this embodiment, hexamethyldisiloxane is used as the raw
成膜されたシリコン−酸素−炭素の複合膜の膜厚は場所により異なり、０．０５μｍ〜０．４μｍ程度の厚みに成膜されていた。また、オージェ電子分光法により分析した水素以外の膜組成は、Ｓｉが約５０ａｔ％、Ｃが約４０ａｔ％、Ｏが約１０ａｔ％であった。 The film thickness of the silicon-oxygen-carbon composite film formed varies depending on the location, and is formed to a thickness of about 0.05 μm to 0.4 μm. The film composition other than hydrogen analyzed by Auger electron spectroscopy was about 50 at% for Si, about 40 at% for C, and about 10 at% for O.
次に、本実施例でシリコン−酸素−炭素の複合膜を成膜した真空容器の排気特性を図２に示す。図２は、相対湿度５０％の大気に１時間曝露した後、排気開始からの真空容器の圧力変化である。
同図（Ａ）に本発明のシリコン−酸素−炭素の複合膜を成膜した真空容器、同図（Ｂ）に比較のためにシリコン−酸素−炭素の複合膜が成膜される前の真空容器、同図（Ｃ）にＴｉＮを成膜した真空容器及び同図（Ｄ）にマグネトロンスパッタ法でＳｉを成膜した真空容器の各測定値をプロットしたものを示した。
図２より、本発明のシリコン−酸素−炭素の複合膜が成膜された真空容器は、成膜する前の電解研磨されたステンレス鋼容器に比べ圧力降下速度が約１０倍に大きくなっていることが明らかとなった。また、ＴｉＮ成膜によっても電解研磨したステンレス鋼に比べて若干圧力降下速度が増大するが、そのＴｉＮ成膜に比べても、本発明のシリコン−酸素−炭素の複合膜の効果が大きいことは明らかである。また、マグネトロンスパッタ法と比較すると圧力降下速度は同等であるが、本発明は気化させた化合物を原料としているため固体を原料とするスパッタ法よりも複雑形状に容易に成膜できる点において優れている。
Next, FIG. 2 shows the exhaust characteristics of the vacuum vessel in which a silicon-oxygen-carbon composite film was formed in this example. FIG. 2 shows the pressure change in the vacuum vessel from the start of exhaustion after exposure to an atmosphere with a relative humidity of 50% for 1 hour.
FIG. 6A shows a vacuum container in which the silicon-oxygen-carbon composite film of the present invention is formed, and FIG. 6B shows a vacuum before the silicon-oxygen-carbon composite film is formed for comparison. The measured values of the container, the vacuum container in which TiN is formed in the figure (C), and the vacuum container in which Si is formed by the magnetron sputtering method are plotted in FIG. (D).
As shown in FIG. 2, the vacuum container on which the silicon-oxygen-carbon composite film of the present invention was formed has a pressure drop rate about 10 times larger than that of the stainless steel container that has been electropolished before film formation. It became clear. The TiN film formation also increases the pressure drop rate slightly compared to the electropolished stainless steel, but the effect of the silicon-oxygen-carbon composite film of the present invention is greater than that of the TiN film formation. it is obvious. In addition, the pressure drop rate is equivalent to that of the magnetron sputtering method, but the present invention is superior in that it can be easily formed into a complicated shape compared to the sputtering method using a solid material as a raw material because the present invention uses a vaporized compound as a raw material. Yes.
本実施例では、原料に気化したヘキサメチルジシロキサンを用いたが、窒素を含有するヘキサメチルジシラザンでも同様の特性が得られた。このとき成膜したＳｉ−Ｃ−Ｎ膜の水素以外の組成は、Ｓｉが約５０ａｔ％、Ｃが約４０ａｔ％、Ｎが約１０ａｔ％であった。 In this example, vaporized hexamethyldisiloxane was used as a raw material, but similar characteristics were obtained with hexamethyldisilazane containing nitrogen. The composition other than hydrogen of the Si—C—N film formed at this time was about 50 at% Si, about 40 at% C, and about 10 at% N.
また、本実施例では直流電流を用いたが、交流電流を用いてもよい。 In this embodiment, a direct current is used, but an alternating current may be used.
このように、本実施例では、ステンレス鋼の表面をシリコン−酸素−炭素の複合膜に置き換えることで室温での水の脱離速度を速くすることができる。 Thus, in this embodiment, the water desorption rate at room temperature can be increased by replacing the surface of stainless steel with a silicon-oxygen-carbon composite film.
図１に示すものでは成膜されるものは真空容器であったが、真空容器の中に入れる部品を真空容器の代わりに（真空）処理容器内に収容するようにしてもよい。 In the case shown in FIG. 1, the film to be formed is a vacuum container. However, a part to be placed in the vacuum container may be accommodated in a (vacuum) processing container instead of the vacuum container.
図３は、図１の方法で被処理真空容器１の内壁に成膜されやすいように補助電極を用いたものである。
図３において、１は表面にシリコン化合物の成膜をされる真空容器、２は電流導入端子、３は直流電源、４は原料のシリコン化合物、５はマスフローコントローラー、６は圧力計、７は成膜を行うための容器、８は可変コンダクタンスバルブである。
FIG. 3 shows an example in which an auxiliary electrode is used so that a film can be easily formed on the inner wall of the
In FIG. 3, 1 is a vacuum vessel in which a silicon compound film is formed on the surface, 2 is a current introduction terminal, 3 is a DC power source, 4 is a raw material silicon compound, 5 is a mass flow controller, 6 is a pressure gauge, and 7 is a component. A container for carrying out the membrane, 8 is a variable conductance valve.
図４は、図１の成膜されるものをアース電位にした場合の実施例である。
図４において、１は表面にシリコン化合物の成膜をされる真空容器、２は電流導入端子、３は直流電源、４は原料のシリコン化合物、５はマスフローコントローラー、６は圧力計、７は成膜を行うための容器、８は可変コンダクタンスバルブである。
FIG. 4 shows an embodiment in which the film to be formed shown in FIG.
In FIG. 4, 1 is a vacuum vessel in which a silicon compound film is formed on the surface, 2 is a current introduction terminal, 3 is a DC power source, 4 is a raw material silicon compound, 5 is a mass flow controller, 6 is a pressure gauge, and 7 is a component. A container for carrying out the membrane, 8 is a variable conductance valve.
図１、図３乃至図４の各実施例において、いずれの場合も、Ａｒ等の不活性ガスを導入するガスラインを設けて、Ｓｉ−Ｃ成膜と同様な方法でＡｒ等の不活性ガスによるプラズマを生成させることでＳｉ−Ｃ膜の成膜前に表面のクリーニングを行うことができる。 1 and 3 to 4, in any case, a gas line for introducing an inert gas such as Ar is provided, and an inert gas such as Ar is formed in the same manner as in the Si—C film formation. The surface can be cleaned before the formation of the Si—C film by generating the plasma.
本発明によれば、真空容器の表面及び部品表面の全面にガス放出の少ない均質な膜を形成することができ、ガス放出の少ない均質な膜を備えた真空容器類を提供できる。 ADVANTAGE OF THE INVENTION According to this invention, a homogeneous film | membrane with little gas emission can be formed in the whole surface of a vacuum vessel surface and component surfaces, and vacuum containers provided with the homogeneous film | membrane with little gas emission can be provided.
１ 被処理真空容器
２ 電流導入端子
３ 直流電源
４ 原料のシリコン化合物
５ マスフローコントローラー
６ 圧力計
７ （真空）処理容器
８ 可変コンダクタンスバルブ
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