JP2006275551A - Evaluation method of contamination state of substrate-manufacturing local space - Google Patents

Evaluation method of contamination state of substrate-manufacturing local space Download PDF

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JP2006275551A
JP2006275551A JP2005090812A JP2005090812A JP2006275551A JP 2006275551 A JP2006275551 A JP 2006275551A JP 2005090812 A JP2005090812 A JP 2005090812A JP 2005090812 A JP2005090812 A JP 2005090812A JP 2006275551 A JP2006275551 A JP 2006275551A
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substrate
adsorbent
local space
space
contamination state
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Toshikazu Taira
敏和 平
Hiroshi Fujii
博史 藤井
Yasuko Sakamoto
保子 坂本
Takaaki Sakakibara
孝明 榊原
Mikio Hasegawa
幹男 長谷川
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Sumika Chemical Analysis Service Ltd
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Sumika Chemical Analysis Service Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for evaluating accurately the contamination state of a local space passed by a substrate at the substrate manufacturing time. <P>SOLUTION: This evaluation method of the contamination state of the local space in a substrate manufacturing process has characteristics, wherein in the substrate manufacturing process, a passive sampler is put into the local space passed by the substrate, and contaminants in the space are collected into an adsorbent in the passive sampler, and then the adsorbed contaminant is eliminated from the adsorbent, and the eliminated contaminant is analyzed. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、基板製造時に該基板が経由する局所的なクリーン空間における汚染状態の評価方法に関するものである。   The present invention relates to a method for evaluating a contamination state in a local clean space through which a substrate passes during manufacture of the substrate.

半導体ウェーハ、液晶基板、磁気ディスク等の電子基板(以下、基板と称する。)を用いた機器の製造においては、その製造空間中の有機物等の汚染物質が基板に吸着する等して、製品の歩留まりの低下や品質の低下が生ずることから、このような機器を製造する工程は、クリーンルームで行われている。そして、各製造過程でのクリーンルームにおける上記有機物等による汚染状態を評価することが必要であるところ、その手法としては、例えば、吸引ポンプで吸引したクリーンルーム内の空気を一定の流量で吸着剤に通し、該空気中の汚染物質を吸着剤に捕集し、捕集された汚染物質を分析する方法が提案されている(例えば、非特許文献1参照。)。   In the manufacture of equipment using electronic substrates (hereinafter referred to as substrates) such as semiconductor wafers, liquid crystal substrates, magnetic disks, etc., contaminants such as organic substances in the manufacturing space are adsorbed on the substrate, and so on. Since the yield and quality are lowered, the process for manufacturing such a device is performed in a clean room. Then, it is necessary to evaluate the state of contamination due to the organic matter etc. in the clean room in each manufacturing process. For example, the air in the clean room sucked by the suction pump is passed through the adsorbent at a constant flow rate. A method has been proposed in which contaminants in the air are collected in an adsorbent and the collected contaminants are analyzed (see, for example, Non-Patent Document 1).

ところで、近年、基板回路の微細化の進行に相俟って、クリーンルームには、より高度な洗浄空間の確保が求められており、また、基板の大型化に伴い、大規模のクリーンルームが必要となってきている。昨今では、このような清浄度の高い空間の確保のためのコスト節約手段として、局所クリーン方式の採用が提案されている。例えば、上記機器の一連の製造における各クリーンルーム内での各種加工処理工程の間に、FOUP(Front Opening Unified Pod)、SMIF(Standard Mechanical Interface)ポッド等の可搬式で密閉可能な基板搬送容器を介在させ、該容器およびそれに装着されるEFEM(Equipment Front End Module)によって局所的なクリーン空間を保持しながら、各工程で処理された基板を該基板搬送容器に収納し、次工程へ搬送する方法が提案されている。   By the way, in recent years, with the progress of miniaturization of substrate circuits, it has been demanded that a clean room has a higher level of cleaning space, and with the increase in size of substrates, a large-scale clean room is required. It has become to. In recent years, the use of a local clean method has been proposed as a cost saving means for securing such a clean space. For example, a portable and airtight substrate transport container such as a FOUP (Front Opening Unified Pod) or SMIF (Standard Mechanical Interface) pod is interposed between various processing processes in each clean room in a series of manufacturing of the above equipment. The substrate and the EFEM (Equipment Front End Module) attached to the container hold a local clean space, and the substrate processed in each process is stored in the substrate transport container and transported to the next process. Proposed.

そして、各工程に介在させる上記の基板搬送容器や装着部品については、これにより形成される局所的な空間の汚染状態を評価することが必要であるところ、その手法としては、例えば、基板搬送容器内に半導体ウェーハ等の収納物を収納し、保管ないし移送を所定時間行った後、基板搬送容器から収納物を取り出し、次に、該収納物の表面に付着した汚染物質を脱離させて、脱離した汚染物質を測定する方法が提案されている(例えば、特許文献1参照。)。   And about said board | substrate conveyance container and mounting components intervened in each process, it is necessary to evaluate the contamination state of the local space formed by this, For example, as a technique, a board | substrate conveyance container is used. After storing a stored item such as a semiconductor wafer in a storage or transfer for a predetermined time, take out the stored item from the substrate transfer container, and then desorb the contaminants attached to the surface of the stored item, A method for measuring the desorbed contaminant has been proposed (see, for example, Patent Document 1).

「付属書3 クリーンルームおよび関連する制御環境空気中の有機物質の測定方法」,JACA No.35A−2003 クリーンルームおよび関連する制御環境中における分子状汚染物質に関する空気清浄度の表記方法および測定方法指針,社団法人 日本空気清浄協会,平成15年3月1日,p.9−12“Appendix 3 Method for Measuring Organic Substances in Cleanroom and Related Control Environment Air”, JACA No. 35A-2003 Air Cleanliness Notation and Measurement Method Guidelines for Molecular Contaminants in Cleanrooms and Related Control Environments, Japan Air Cleaners Association, March 1, 2003, p. 9-12 特開2004−340685号公報Japanese Patent Laid-Open No. 2004-340685

しかしながら、FOUPやSMIFポッド、EFEMは、クリーンルーム内に比べて空間体積は遥かに小さく密閉系であり、ポンプを用いて吸引、捕集することが難しく、また、上記のような汚染状態の評価方法では、吸着剤に捕集される汚染物質の量が、吸着剤を通した大気中に含まれる汚染物質の量に対して少なくなることがあり、その結果、例えば、汚染物質の量が少ない局所的空間の汚染物質の定量分析においては、分析値が定量下限値を下回ること等があり、汚染状態の評価の精度は、充分満足のいくものではなかった。
かかる状況のもと、本発明が解決しようとする課題は、基板製造時に、該基板が経由する局所的な空間の汚染状態を精度よく評価する方法を提供することにある。
However, FOUP, SMIF pod, and EFEM have a much smaller space volume than a clean room and are sealed systems, and it is difficult to suck and collect using a pump. In this case, the amount of pollutants collected by the adsorbent may be smaller than the amount of pollutants contained in the atmosphere through the adsorbent. In the quantitative analysis of pollutants in the target space, the analytical value may fall below the lower limit of quantification, and the accuracy of the assessment of the contamination state was not fully satisfactory.
Under such circumstances, the problem to be solved by the present invention is to provide a method for accurately evaluating the contamination state of a local space through which the substrate passes during the manufacture of the substrate.

すなわち、本発明は、基板製造工程において、該基板が経由する局所的空間にパッシブサンプラーを入れ、当該空間内の汚染物質を該パッシブサンプラー内の吸着剤に捕集し、次に、該吸着剤から吸着された汚染物質を脱離させ、脱離した汚染物質を分析することを特徴とする該局所空間の汚染状態の評価方法にかかるものである。   That is, according to the present invention, in the substrate manufacturing process, a passive sampler is placed in a local space through which the substrate passes, and contaminants in the space are collected in an adsorbent in the passive sampler. The present invention relates to a method for evaluating the contamination state of the local space, characterized in that the adsorbed contaminant is desorbed from the sample and the desorbed contaminant is analyzed.

本発明方法により、基板製造工程における局所空間の汚染状況を精度よく評価することができ、本方法は、基板製造設備内における清浄空間の確保に有用である。   According to the method of the present invention, the contamination state of the local space in the substrate manufacturing process can be accurately evaluated, and this method is useful for securing a clean space in the substrate manufacturing facility.

本発明に係る基板製造工程における局所空間とは、半導体ウェーハ、液晶基板、磁気ディスク等の基板の製造時に、これらの基板が経由する局所的な空間であって、SEMI(Semiconductor Equipment and Materials International)規格に定められたFOUP(Front Opening Unified Pod)、SMIF(Standard Mechanical Interface )ポッド、EFEM(Equipment Front End Module)、特開2000−58633号公報や特開2001−85507号公報等に記載された基板搬送容器やその装着部品等があげられる。   The local space in the substrate manufacturing process according to the present invention is a local space through which these substrates pass when manufacturing substrates such as semiconductor wafers, liquid crystal substrates, and magnetic disks, and is SEMI (Semiconductor Equipment and Materials International). Standard FOUP (Front Opening Unified Pod), SMIF (Standard Mechanical Interface) pod, EFEM (Equipment Front End Module), substrates described in JP 2000-58633 A, JP 2001-85507 A, etc. Examples include a transport container and its mounting parts.

本発明のパッシブサンプラーとしては、通常、気体透過性の膜からなる容器に吸着剤を充填した装置が用いられる。該気体透過性の膜には、分析の対象となる汚染物質の分析に影響を与えない材質を用いることが好ましく、通常、ポリエチレンなどのポリオレフィン樹脂、ポリエステル樹脂、フッ素樹脂などの粒子を焼結あるいは溶結したものが用いられる。好ましくは、フッ素樹脂製の膜である。また、該吸着剤としては、多孔質高分子系吸着剤、グラファイトカーボン系吸着剤、活性炭などが用いられる。   As the passive sampler of the present invention, an apparatus in which a container made of a gas permeable membrane is filled with an adsorbent is usually used. The gas permeable membrane is preferably made of a material that does not affect the analysis of the pollutant to be analyzed. Usually, particles such as polyolefin resin such as polyethylene, polyester resin, and fluororesin are sintered or What was welded is used. Preferably, it is a fluororesin film. As the adsorbent, a porous polymer adsorbent, a graphite carbon adsorbent, activated carbon, or the like is used.

パッシブサンプラーとしては、例えば、特開2002−5797号公報、特開2002−357517号公報、特開2004−191120号公報等に記載の装置があげられる。また、市販品(例えば、スペルコジャパン社製、商品名「VOC−TD」等。)を用いてもよい。   Examples of the passive sampler include devices described in JP-A No. 2002-5797, JP-A No. 2002-357517, JP-A No. 2004-191120, and the like. Moreover, you may use a commercial item (For example, the sperco Japan company make, brand name "VOC-TD" etc.).

パッシブサンプラーの使用においては、気体透過性の膜からなる容器を、あらかじめ、アセトンやヘキサン等の有機溶剤、純水等で十分に洗浄し、乾燥しておくことが好ましい。また、あらかじめ、吸着剤を熱処理、例えば、不活性ガスを通気しながら吸着剤を300℃以上に加熱する処理を行うことが好ましい。なお、ここで不活性ガスとは、分析の対象となる汚染物質の分析に影響を及ぼさないガスを意味し、分析対象の汚染物質の種類にもよるが、そのようなガスとしては、窒素、アルゴン、ヘリウムなどの不活性ガス;空気などが用いられる。   In the use of a passive sampler, it is preferable that a container made of a gas permeable membrane is sufficiently washed beforehand with an organic solvent such as acetone or hexane, pure water, etc. and dried. In addition, it is preferable to perform in advance a heat treatment of the adsorbent, for example, a process of heating the adsorbent to 300 ° C. or higher while passing an inert gas. Here, the inert gas means a gas that does not affect the analysis of the pollutant to be analyzed, and depending on the type of pollutant to be analyzed, such gas includes nitrogen, An inert gas such as argon or helium; air or the like is used.

上記の局所空間内のパッシブサンプラーの滞留時間、即ち、当該空間内の汚染物質を捕集するに要する時間としては、通常2〜24時間であり、好ましくは10〜24時間である。   The residence time of the passive sampler in the local space, that is, the time required to collect the contaminants in the space is usually 2 to 24 hours, preferably 10 to 24 hours.

パッシブサンプラーに捕集された汚染物質の分析では、パッシブサンプラーから吸着剤を取り出し、加熱脱離法あるいは溶剤抽出法により、吸着剤から汚染物質を脱離させ、脱離した汚染物質を公知の方法により分析する。   In the analysis of pollutants collected by the passive sampler, the adsorbent is taken out from the passive sampler, and the pollutant is desorbed from the adsorbent by the thermal desorption method or solvent extraction method. Analyze by.

加熱脱離法は、例えば、市販の加熱脱離管に吸着剤を移し、該加熱脱離管を加熱し、不活性ガスを通気することにより行う。加熱脱離を行う温度および時間は、分析対象となる汚染物質により異なるが、加熱脱離温度としては、通常250〜350℃であり、好ましくは250〜300℃である。また、加熱脱離時間は、通常10分間以上であり、好ましくは20分間程度である。一方、溶剤抽出法は、例えば、パッシブサンプラーから取り出した吸着剤を溶剤に入れ、該吸着剤から汚染物質を抽出、溶出させる。該溶剤は分析対象となる汚染物質により適宜選択される。   The heat desorption method is performed, for example, by transferring the adsorbent to a commercially available heat desorption tube, heating the heat desorption tube, and venting an inert gas. The temperature and time for performing the heat desorption vary depending on the contaminant to be analyzed, but the heat desorption temperature is usually 250 to 350 ° C., preferably 250 to 300 ° C. The heat desorption time is usually 10 minutes or more, preferably about 20 minutes. On the other hand, in the solvent extraction method, for example, an adsorbent taken out from a passive sampler is put in a solvent, and contaminants are extracted and eluted from the adsorbent. The solvent is appropriately selected depending on the contaminant to be analyzed.

吸着剤から脱離した汚染物質の分析方法としては、公知の方法が用いられ、加熱脱離法では、例えば、ガスクロマトグラフ(GC)法、ガスクロマトグラフ−質量分析(GC−MS)法等があげられ、溶剤抽出法では、例えば、ガスクロマトグラフ(GC)法、液体クロマトグラフ(LC)法、ガスクロマトグラフ−質量分析(GC−MS)法、キャピラリー電気泳動(CE)法等があげられる。好ましくはGC−MS法である。また、上記分析においては、吸着剤から脱離させた汚染物質を、必要に応じ、汚染物質を含むガスを液体窒素等の冷媒で冷却した管に導入して汚染物質を凝縮させる、汚染物質を含む液を濃縮する等の濃縮処理を行った後に分析してもよい。   As a method for analyzing the contaminants desorbed from the adsorbent, a known method is used. Examples of the thermal desorption method include a gas chromatograph (GC) method and a gas chromatograph-mass spectrometry (GC-MS) method. Examples of the solvent extraction method include a gas chromatograph (GC) method, a liquid chromatograph (LC) method, a gas chromatograph-mass spectrometry (GC-MS) method, and a capillary electrophoresis (CE) method. The GC-MS method is preferred. In the above analysis, the pollutant desorbed from the adsorbent is introduced into a tube cooled with a refrigerant such as liquid nitrogen as necessary to condense the pollutant. You may analyze after performing the concentration process of concentrating the liquid containing.

本発明方法により、基板製造工程における局所空間の汚染状況を精度よく評価することができ、本方法は、基板製造設備内における清浄空間の確保に有用である。特に、本発明は、汚染物質の量が少ないFOUP(Front Opening Unified Pod)、SMIF(Standard Mechanical Interface )ポッド、EFEM(Equipment Front End Module)等の基板搬送容器やその装着部品により形成される局所的空間の汚染状態の評価に有用である。   According to the method of the present invention, the contamination state of the local space in the substrate manufacturing process can be accurately evaluated, and this method is useful for securing a clean space in the substrate manufacturing facility. In particular, the present invention is a local form formed by a substrate transport container such as a FOUP (Front Opening Unified Pod), SMIF (Standard Mechanical Interface) pod, EFEM (Equipment Front End Module) or the like and a mounting part thereof with a small amount of contaminants. Useful for assessing the pollution status of a space.

本発明を、実施例によりさらに詳しく説明する。   The invention is explained in more detail by means of examples.

(実施例1)
パッシブサンプラー(スペルコジャパン製、商品名「VOC−TD」、吸着剤:グラファイトカーボン系吸着剤)をクリーンルーム内に24時間放置し、クリーンルーム内の空気中の有機物質をパッシブサンプラーに捕集した。次に、パッシブサンプラーから吸着剤を直径6mm×16cmのガラスチューブに移しいれ、加熱脱離濃縮装置(GLサイエンス社製、CP4020型)にセットして300℃で10分間加熱脱離処理し、発生したガスを液体窒素で濃縮処理し、ガスクロマトグラフ−質量分析計(アジレントテクノロジ社製、HP−5973N型)で分析した。分析結果を表1に示す。なお、検出された有機物質について、その総量をトルエン換算の量として表した。
Example 1
A passive sampler (manufactured by Spelco Japan, trade name “VOC-TD”, adsorbent: graphite carbon-based adsorbent) was left in a clean room for 24 hours, and organic substances in the air in the clean room were collected by a passive sampler. Next, the adsorbent is transferred from the passive sampler to a glass tube with a diameter of 6 mm x 16 cm, set in a heat desorption concentrator (GL Science, CP4020 type), and heated and desorbed at 300 ° C for 10 minutes. The gas was concentrated with liquid nitrogen and analyzed with a gas chromatograph-mass spectrometer (HP-5993N type, manufactured by Agilent Technologies). The analysis results are shown in Table 1. In addition, about the detected organic substance, the total amount was represented as the amount of toluene conversion.

(比較例1)
吸引ポンプを用いて、グラファイトカーボン系吸着剤を90mg充填した捕集管(直径6mm×長さ16cm)に、クリーンルーム内の空気を0.1L/分の流量で24時間通し、クリーンルーム内の大気中の有機物質を捕集管に捕集した。次に、捕集管から吸着剤を直径6mm×16cmのガラスチューブに移しいれ、加熱脱離濃縮装置(GLサイエンス社製、CP4020型)にセットして300℃で10分間加熱脱離処理し、発生したガスを液体窒素で濃縮処理し、ガスクロマトグラフ−質量分析計(アジレントテクノロジ社製、HP−5973N型)で分析した。分析結果を表1に示す。なお、検出された有機物質について、その総量をトルエン換算の量として表した。
(Comparative Example 1)
Using a suction pump, air in the clean room was passed through a collection tube (diameter 6 mm x length 16 cm) filled with 90 mg of graphite carbon-based adsorbent at a flow rate of 0.1 L / min for 24 hours. Of organic material was collected in a collection tube. Next, the adsorbent is transferred from the collection tube to a glass tube having a diameter of 6 mm × 16 cm, set in a heat desorption concentrator (GL Science, CP4020 type), and heat desorbed at 300 ° C. for 10 minutes. The generated gas was concentrated with liquid nitrogen and analyzed with a gas chromatograph-mass spectrometer (HP-5993N type, manufactured by Agilent Technologies). The analysis results are shown in Table 1. In addition, about the detected organic substance, the total amount was represented as the amount of toluene conversion.

Figure 2006275551
Figure 2006275551

Claims (1)

基板製造工程において、該基板が経由する局所的空間にパッシブサンプラーを入れ、当該空間内の汚染物質を該パッシブサンプラー内の吸着剤に捕集し、次に、該吸着剤から吸着された汚染物質を脱離させ、脱離した汚染物質を分析することを特徴とする基板製造工程における局所空間の汚染状態の評価方法。

In the substrate manufacturing process, a passive sampler is placed in a local space through which the substrate passes, and the contaminant in the space is collected in the adsorbent in the passive sampler, and then the contaminant adsorbed from the adsorbent. A method for evaluating a contamination state of a local space in a substrate manufacturing process, wherein the desorbed material is desorbed and the desorbed contaminant is analyzed.

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