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JP3622034B2 - Surface treatment method for vacuum deposition film forming chamber - Google Patents

Surface treatment method for vacuum deposition film forming chamber Download PDF

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Publication number
JP3622034B2
JP3622034B2 JP00689695A JP689695A JP3622034B2 JP 3622034 B2 JP3622034 B2 JP 3622034B2 JP 00689695 A JP00689695 A JP 00689695A JP 689695 A JP689695 A JP 689695A JP 3622034 B2 JP3622034 B2 JP 3622034B2
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Japan
Prior art keywords
film forming
forming chamber
vacuum deposition
deposition film
vacuum
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 - Fee Related
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JP00689695A
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Japanese (ja)
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JPH08199334A (en
Inventor
貞一郎 鮫島
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Neos Co Ltd
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Neos Co Ltd
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Description

【0001】
【産業上の利用分野】
本発明は、真空蒸着膜形成室の表面処理方法及び真空蒸着膜形成室に関する。
【0002】
【従来の技術】
半導体、液晶製造分野を始め、真空蒸着を行う産業においては、例えばシリコンウエハ、ガラス基板、工具類といった本来の被蒸着物の表面に、種々の物質をコーティングすることを目的としているが、SiO、ITO等の蒸着物質は、被蒸着物以外の真空蒸着膜形成室の表面にも同時に蒸着し、これを防ぐことはできない。本来コーティングを目的とする被蒸着物は、所定量を蒸着すれば真空容器内部より取り出され、さらに新しい被蒸着物が真空容器内に持ち込まれ、蒸着が行われる。この作業が繰り返されるため、真空蒸着膜形成室の内部部品表面には、蒸着物が徐々に堆積していくことになる。
【0003】
蒸着物がSiO、ITO等の無機質の場合、真空蒸着膜形成室の内部部品に使われる金属材料(主に、ステンレススチール、アルミニウム合金、チタン等)との密着性が十分ではなく、SiO、ITO等の蒸着物の付着量が増加するに従って、蒸着膜内部に堆積される内部応力によって剥離現象が生じる。
【0004】
いったん、堆積した膜が剥離すると、これらはパーティクル化し、本来の被蒸着物表面を汚染するとともにその品質を劣化させる。半導体や液晶製造時における不良品発生の原因は、このパーティクルによるところが大きい。
【0005】
この際、膜剥離によるパーティクルを抑制するために、真空蒸着装置内部に蒸着物が厚く付着する(剥離膜厚に達する)前に真空蒸着装置内部の部品表面を洗浄し、付着した蒸着物を除去することが従来行われてきた。
【0006】
SiOやITOを蒸着する場合、他の蒸着物(例えば、アルミニウム、ニッケル。タングステン等)に比べ、より膜厚が小さいにもかかわらず剥離現象が生じる。かかる場合、頻繁に真空蒸着装置の運転を中断し、部品を洗浄、交換しなければならず、装置の稼働率を著しく低下させることになる。
【0007】
従来、いったん付着したSiOやITOは化学薬品或いはブラスト等によって除去される。また、膜剥離を抑制するため、ブラストや熔射等によって表面を粗面化する方法が一般的に採用されている。
【0008】
パーティクルを原因とする不良品の発生率が高い真空蒸着の場合、部品表面に付着したパーティクルが真空容器内部に持ち込まれることは極力抑制されなければならない。しかしながら、化学洗浄や特にブラスト処理、熔射処理、を施された表面には膨大な数のパーティクルが付着するため、純水中で超音波洗浄等によって清浄化しなくてはならない。
【0009】
純水による洗浄工程はもちろん、水と直接接触しない場合でも、大気に晒すだけでも部品表面には水分が吸着される。吸着された水分は、従来はベーキングと呼ばれる加熱処理により除去されていた。ベーキング工程では、付着水の完全なる除去は困難であり、ベーキング装置から取り出したときに、再び空気中の水分が吸着されるので、実質的には表面に水分を残したまま真空容器内に戻されることは避けられなかった。
【0010】
SiOやITOの場合、表面に付着する水分が多いほど剥離しやすい傾向にあるが、従来は、表面の粗面化、或いはベーキングによる水分除去しか行われていない。このため、他の蒸着物に比べて、SiOやITOの場合不良品の発生率が高く、また、部品の洗浄も頻繁に行われていた。
【0011】
【発明が解決しようとする課題】
本発明は、真空蒸着膜形成室に付着するパーティクルを無くすとともに、蒸着物の剥離を抑制し、不良品の発生率を抑制するための真空蒸着膜形成室の処理方法及び真空蒸着膜形成室を提供することを目的とする。
【0012】
【課題を解決するための手段】
本発明は、以下の真空蒸着膜形成室の処理方法を提供するものである。
【0013】
1. 真空蒸着膜形成室をシラン化合物によりコーティングすることを特徴とする真空蒸着膜形成室の表面処理方法。
【0014】
2. 真空蒸着膜形成室に金属熔射膜を形成し、該金属熔射膜をシラン化合物によりコーティングすることを特徴とする真空蒸着膜形成室の表面処理方法。
【0015】
3. 真空蒸着膜形成室に金属熔射膜層及びシランコーティング層をこの順に積層してなる真空蒸着膜形成室。
【0016】
本発明において、シラン化合物としては、以下の化合物が例示される:
(1) フッ素化されていてもよいアルコキシシラン類:トリメチルメトキシシラン、トリメチルエトキシシラン、テトラメトキシシラン、メチルトリエトキシシラン、テトラエトキシシラン、メチルジメトキシシラン、メチルジエトキシシラン、ジメチルエトキシシラン、トリメトキシトリフルオロプロピルシランなど;
(2) フッ素化されていてもよいクロロシラン類:トリメチルクロロシラン、ジメチルジクロロシラン、ジメチルクロロシラン、ジメチルトリフルオロメチルクロロシランなど;
(3) フッ素化されていてもよいシラザン類:ヘキサメチルジシラザン、サイクリックシラザン混合物(〔MeSiNH〕、n=3〜4)、ジメチルトリメチルシリルアミン、ジエチルトリメチルシリルアミン、ジメチルトリ(トリフルオロメチル)シリルアミンなど。
【0017】
好ましいシラン化合物として、トリメチルメトキシシラン、トリメチルクロロシラン、ヘキサメチルジシラザンが挙げられる。
【0018】
熔射される金属としては、アルミニウム(Al)、チタン(Ti)、銅(Cu)、モリブデン(Mo)等が挙げられる。
【0019】
真空蒸着膜形成室としては、シリコンウエハ、ガラス基板、工具類などの被蒸着物が蒸着される際に、該被蒸着物が収容される部屋を意味する。該真空蒸着膜形成室の表面は、蒸着物が付着する可能性のあるものであり、真空蒸着膜形成室を構成する内部部品としては、防着板、マスク、ホルダー、トレイ等が挙げられる。真空蒸着膜形成室は、従来の真空蒸着の際に形成されていたものがそのまま用いられる。
【0020】
金属の熔射及びシラン化合物のコーティングは、各々公知の方法により容易に真空蒸着膜形成室表面に形成することができる。
【0021】
真空蒸着膜形成室の内面を構成する各部品表面は、熔射またはシラン化合物のコーティング処理に先立ち、クロム酸等で前処理するのが好ましい。
【0022】
なお、コーティングは、SiOの蒸着物に対しては特にシラン化合物を用いるのが好ましいが、ITO(インジウム・錫オキシド)を蒸着させる場合にはシラン化合物の代わりに、又はシラン化合物とともにチタン化合物、インジウム化合物、錫化合物によりコーティングするのが好ましい。
【0023】
また、シリコンウエハなどへの真空蒸着方法自体も、従来公知の方法がそのまま本発明に適用される。
【0024】
【発明の効果】
本発明によれば、パーティクルや剥離した薄膜により蒸着製品が汚染される可能性が大幅に軽減され、不良品の発生率が大きく低下する。
【0025】
【実施例】
以下、本発明を実施例とともに説明するが、本発明がこれら実施例に限定されないことはいうまでもない。
【0026】
実施例1〜13及び比較例1〜4
SiOターゲットを取り付けたスパッタ装置にて、種々の材質(SUS304、AlまたはTi)の蒸着膜形成室の部品に薄膜を形成させ、膜の付着状況を観察した。各種の条件及び剥離性を表1に示す。
【0027】
なお、ブラストは、メディヤ材としてAlを用い、圧力4.5kg/cmの条件で行った。また、熔射は、プラズマ熔射により行い、膜厚は150ミクロンであった。
【0028】
また、スパッタ条件は、出力(240W・Hr)、造膜速度(1.25μm/Hr)であった。
【0029】
さらに、表面処理は、デップコート後、200℃で1時間ベーキングした。
【0030】
表1中の表面処理剤の記号は、以下の通りである。
【0031】
TMMS:トリメチルメトキシシラン
TMCS:トリメチルクロロシラン
HMDS:ヘキサメチルジシラザン
TMTFS:トリメトキシトリフルオロプロピルシラン
【0032】
【表1】

Figure 0003622034
実施例14〜16及び比較例5〜7
SiOターゲットの代わりにITOターゲットを用いた他は上記実施例1〜13及び比較例1〜4と同様にして薄膜の付着状況を観察した。結果を表2に示す。
【0033】
【表2】
Figure 0003622034
実施例20〜25及び比較例8〜10
SiOターゲットを取り付けたスパッタ装置を用いる代わりに、プラズマCVD装置内でテトラエトキシシラン(TEOS)を用いてSiOの薄膜を形成した以外は、実施例1と同様にして薄膜の付着状況を観察した。結果を表3に示す。
【0034】
なお、プラズマCVD装置による造膜速度は、3μm/Hrであった。
【0035】
【表3】
Figure 0003622034
[0001]
[Industrial application fields]
The present invention relates to a surface treatment method for a vacuum vapor deposition film forming chamber and a vacuum vapor deposition film forming chamber.
[0002]
[Prior art]
Semiconductor, began LCD manufacturing field, and in the industry for performing vacuum deposition, for example a silicon wafer, a glass substrate, the surface of the original evaporation object such tools include, but are intended to coat various materials, SiO 2 The deposition material such as ITO is deposited on the surface of the vacuum deposition film forming chamber other than the deposition object at the same time, and this cannot be prevented. The deposition object originally intended for coating is taken out from the inside of the vacuum container when a predetermined amount is deposited, and a new deposition object is brought into the vacuum container to perform deposition. Since this operation is repeated, the vapor deposition is gradually deposited on the surface of the internal components of the vacuum vapor deposition film forming chamber.
[0003]
In the case where the deposited material is inorganic such as SiO 2 or ITO, the adhesion to the metal material (mainly stainless steel, aluminum alloy, titanium, etc.) used for the internal parts of the vacuum deposited film forming chamber is not sufficient, and SiO 2 As the deposition amount of the deposited material such as ITO increases, a peeling phenomenon occurs due to the internal stress deposited inside the deposited film.
[0004]
Once the deposited film is peeled off, these particles become particles, contaminating the original surface of the deposition object and deteriorating its quality. The cause of defective products during the manufacture of semiconductors and liquid crystals is largely due to these particles.
[0005]
At this time, in order to suppress particles due to film peeling, the surface of the parts inside the vacuum evaporation system is washed before the deposited material thickly adheres to the inside of the vacuum deposition system (removes the film thickness), and the deposited material is removed It has been done in the past.
[0006]
In the case of depositing SiO 2 or ITO, a peeling phenomenon occurs even though the film thickness is smaller than other deposited materials (for example, aluminum, nickel, tungsten, etc.). In such a case, the operation of the vacuum vapor deposition apparatus must be frequently interrupted to clean and replace the parts, and the operating rate of the apparatus is significantly reduced.
[0007]
Conventionally, once attached SiO 2 and ITO are removed by chemicals or blasting. Moreover, in order to suppress film peeling, the method of roughening the surface by blasting or spraying is generally employed.
[0008]
In the case of vacuum deposition in which the incidence of defective products due to particles is high, it is necessary to suppress as much as possible the particles adhering to the component surface from being brought into the vacuum container. However, since a large number of particles adhere to the surface that has been subjected to chemical cleaning, especially blasting and spraying, it must be cleaned by ultrasonic cleaning or the like in pure water.
[0009]
Even in the case of a cleaning process using pure water, even when it is not in direct contact with water, moisture is adsorbed on the surface of the component even if it is exposed to the atmosphere. The adsorbed moisture has been conventionally removed by a heat treatment called baking. In the baking process, it is difficult to completely remove the adhering water, and moisture in the air is adsorbed again when it is taken out from the baking apparatus. Therefore, it is returned to the vacuum container while leaving moisture on the surface. It was inevitable.
[0010]
In the case of SiO 2 or ITO, the more the moisture adhering to the surface, the easier it is to peel off. Conventionally, however, only the surface is roughened or the moisture is removed by baking. For this reason, in the case of SiO 2 or ITO, the occurrence rate of defective products is high compared to other vapor-deposited materials, and parts are frequently cleaned.
[0011]
[Problems to be solved by the invention]
The present invention eliminates particles adhering to a vacuum vapor deposition film forming chamber, suppresses separation of vapor deposits, and suppresses the occurrence rate of defective products. The purpose is to provide.
[0012]
[Means for Solving the Problems]
The present invention provides the following processing method for a vacuum deposited film forming chamber.
[0013]
1. A surface treatment method for a vacuum deposition film forming chamber, wherein the vacuum deposition film forming chamber is coated with a silane compound.
[0014]
2. A surface treatment method for a vacuum deposition film forming chamber, comprising forming a metal spray film in a vacuum deposition film forming chamber and coating the metal spray film with a silane compound.
[0015]
3. A vacuum deposition film forming chamber formed by laminating a metal spray film layer and a silane coating layer in this order in a vacuum deposition film forming chamber.
[0016]
In the present invention, examples of the silane compound include the following compounds:
(1) Alkoxysilanes which may be fluorinated: trimethylmethoxysilane, trimethylethoxysilane, tetramethoxysilane, methyltriethoxysilane, tetraethoxysilane, methyldimethoxysilane, methyldiethoxysilane, dimethylethoxysilane, trimethoxy Trifluoropropylsilane and the like;
(2) Chlorosilanes which may be fluorinated: trimethylchlorosilane, dimethyldichlorosilane, dimethylchlorosilane, dimethyltrifluoromethylchlorosilane and the like;
(3) Silazanes which may be fluorinated: hexamethyldisilazane, cyclic silazane mixture ([Me 2 SiNH] n , n = 3 to 4), dimethyltrimethylsilylamine, diethyltrimethylsilylamine, dimethyltri (trifluoro Methyl) silylamine and the like.
[0017]
Preferable silane compounds include trimethylmethoxysilane, trimethylchlorosilane, and hexamethyldisilazane.
[0018]
Examples of the metal to be sprayed include aluminum (Al), titanium (Ti), copper (Cu), and molybdenum (Mo).
[0019]
The vacuum deposition film forming chamber means a chamber in which a deposition object such as a silicon wafer, a glass substrate, or tools is deposited when the deposition object is deposited. The surface of the vacuum deposition film forming chamber has a possibility of depositing deposits, and examples of the internal parts constituting the vacuum deposition film forming chamber include a deposition plate, a mask, a holder, and a tray. What was formed in the case of the conventional vacuum evaporation is used as it is for the vacuum evaporation film formation chamber.
[0020]
The metal spray and the silane compound coating can each be easily formed on the surface of the vacuum deposition film forming chamber by a known method.
[0021]
The surface of each part constituting the inner surface of the vacuum vapor deposition film forming chamber is preferably pretreated with chromic acid or the like prior to spraying or coating with a silane compound.
[0022]
In addition, it is preferable to use a silane compound for the SiO 2 deposit, but in the case of depositing ITO (indium / tin oxide), the coating is a titanium compound instead of the silane compound or together with the silane compound, It is preferable to coat with an indium compound or a tin compound.
[0023]
Further, as a vacuum deposition method itself on a silicon wafer or the like, a conventionally known method is applied to the present invention as it is.
[0024]
【The invention's effect】
According to the present invention, the possibility that the deposited product is contaminated by the particles or the peeled thin film is greatly reduced, and the incidence of defective products is greatly reduced.
[0025]
【Example】
EXAMPLES Hereinafter, although this invention is demonstrated with an Example, it cannot be overemphasized that this invention is not limited to these Examples.
[0026]
Examples 1-13 and Comparative Examples 1-4
A thin film was formed on the components in the deposition film forming chamber made of various materials (SUS304, Al or Ti) with a sputtering apparatus equipped with a SiO 2 target, and the state of film adhesion was observed. Various conditions and peelability are shown in Table 1.
[0027]
The blasting was performed using Al 2 O 3 as a media material under a pressure of 4.5 kg / cm 2 . The spraying was performed by plasma spraying, and the film thickness was 150 microns.
[0028]
The sputtering conditions were an output (240 W · Hr) and a film forming speed (1.25 μm / Hr).
[0029]
Furthermore, the surface treatment was baked at 200 ° C. for 1 hour after dip coating.
[0030]
The symbols for the surface treatment agent in Table 1 are as follows.
[0031]
TMMS: Trimethylmethoxysilane TMCS: Trimethylchlorosilane HMDS: Hexamethyldisilazane TMTFS: Trimethoxytrifluoropropylsilane
[Table 1]
Figure 0003622034
Examples 14-16 and Comparative Examples 5-7
The adhesion state of the thin film was observed in the same manner as in Examples 1 to 13 and Comparative Examples 1 to 4 except that an ITO target was used instead of the SiO 2 target. The results are shown in Table 2.
[0033]
[Table 2]
Figure 0003622034
Examples 20-25 and Comparative Examples 8-10
Instead of using the sputtering apparatus with the SiO 2 target attached, the thin film adhesion state was observed in the same manner as in Example 1 except that a thin film of SiO 2 was formed using tetraethoxysilane (TEOS) in the plasma CVD apparatus. did. The results are shown in Table 3.
[0034]
In addition, the film forming speed by the plasma CVD apparatus was 3 μm / Hr.
[0035]
[Table 3]
Figure 0003622034

Claims (3)

真空蒸着膜形成室をシラン化合物によりコーティングすることを特徴とする真空蒸着膜形成室の表面処理方法。A surface treatment method for a vacuum deposition film forming chamber, wherein the vacuum deposition film forming chamber is coated with a silane compound. 真空蒸着膜形成室に金属熔射膜を形成し、該金属熔射膜をシラン化合物によりコーティングすることを特徴とする真空蒸着膜形成室の表面処理方法。A surface treatment method for a vacuum deposition film forming chamber, comprising forming a metal spray film in a vacuum deposition film forming chamber and coating the metal spray film with a silane compound. 真空蒸着膜形成室表面に金属熔射膜層及びシランコーティング層をこの順に積層してなる真空蒸着膜形成室。A vacuum deposition film forming chamber formed by laminating a metal spray film layer and a silane coating layer in this order on the surface of the vacuum deposition film forming chamber.
JP00689695A 1995-01-20 1995-01-20 Surface treatment method for vacuum deposition film forming chamber Expired - Fee Related JP3622034B2 (en)

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KR101090895B1 (en) * 2003-05-09 2011-12-08 에이에스엠 아메리카, 인코포레이티드 Reactor surface passivation through chemical deactivation
CN120174316A (en) * 2025-03-27 2025-06-20 合肥江丰电子材料有限公司 A surface treatment method for the reverse sputtering surface in an aluminum target and a copper backing plate target assembly

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