JP2002307080A - Ultrapure water production equipment - Google Patents
Ultrapure water production equipmentInfo
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- JP2002307080A JP2002307080A JP2001114263A JP2001114263A JP2002307080A JP 2002307080 A JP2002307080 A JP 2002307080A JP 2001114263 A JP2001114263 A JP 2001114263A JP 2001114263 A JP2001114263 A JP 2001114263A JP 2002307080 A JP2002307080 A JP 2002307080A
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- Prior art keywords
- gas
- water
- membrane
- pure water
- chamber
- Prior art date
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- Degasification And Air Bubble Elimination (AREA)
- Physical Water Treatments (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は超純水製造装置に係
り、特に、ウエハ洗浄水として好適な、溶存酸素（Ｄ
Ｏ）濃度はきわめて低いが、適度な溶存ガスを含有する
超純水を製造するための超純水製造装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for producing ultrapure water, and more particularly to an apparatus for dissolving dissolved oxygen (D) suitable as wafer cleaning water.
O) The present invention relates to an ultrapure water producing apparatus for producing ultrapure water having an extremely low concentration but containing an appropriate amount of dissolved gas.
【０００２】[0002]
【従来の技術】従来、半導体のウエハ洗浄水として用い
られている超純水は、図２に示すように前処理システム
１、一次純水システム２及びサブシステム３から構成さ
れる超純水製造装置で原水（工業用水、市水、井水等）
を処理することにより製造されている。即ち、凝集、加
圧浮上（沈殿）、濾過装置等よりなる前処理システム１
で、原水中の懸濁物質やコロイド物質を除去した後、逆
浸透膜分離装置、脱気装置及びイオン交換装置（混床式
又は４床５塔式）を備える一次純水システム２で、原水
中のイオンや有機成分を除去し、熱交換器、低圧紫外線
酸化装置、イオン交換純水装置及び限外濾過膜分離装置
を備えるサブシステム３で、水の純度をより一層高めて
超純水が製造される。このサブシステム３において、低
圧紫外線酸化装置では、低圧紫外線ランプより出される
１８５ｎｍの紫外線によりＴＯＣを有機酸さらにはＣＯ
２まで分解する。生成した有機酸及びＣＯ２は後段のイ
オン交換樹脂で除去される。限外濾過膜分離装置では、
微小粒子が除去されイオン交換樹脂の流出粒子も除去さ
れる。2. Description of the Related Art Conventionally, ultrapure water used as semiconductor wafer cleaning water is manufactured by a pretreatment system 1, a primary pure water system 2 and a subsystem 3 as shown in FIG. Raw water with equipment (industrial water, city water, well water, etc.)
It is manufactured by processing. That is, a pretreatment system 1 including coagulation, pressure flotation (sedimentation), a filtration device, and the like.
After removing suspended substances and colloidal substances in the raw water, the primary purified water system 2 equipped with a reverse osmosis membrane separation device, a degassing device and an ion exchange device (mixed-bed type or four-bed five-column type) is used. The system removes ions and organic components in the water, and further increases the purity of water in the subsystem 3 that includes a heat exchanger, a low-pressure ultraviolet oxidation device, an ion-exchange pure water device, and an ultrafiltration membrane separation device. Manufactured. In this subsystem 3, in the low-pressure ultraviolet oxidation device, TOC is converted into organic acid and CO by ultraviolet light of 185 nm emitted from the low-pressure ultraviolet lamp.
Disassemble to 2 . The generated organic acid and CO 2 are removed by a subsequent ion exchange resin. In ultrafiltration membrane separation equipment,
The fine particles are removed, and the outflow particles of the ion exchange resin are also removed.
【０００３】このような超純水製造装置では、製造され
た超純水をウエハ洗浄水として使用するために、可能な
限りＤＯを除去することが求められており、超純水製造
における最終工程のサブシステムに更に脱気装置を設置
することが多くなってきている。例えば特開平９−２９
２５１号公報には、イオン交換純水装置の後段に膜式脱
気装置を設けてＤＯ濃度を低減することが記載されてい
る。膜式脱気装置は、ガス透過膜で隔てられた気室及び
水室を有し、水室に水を流し、気室を真空ポンプで吸引
して、水中のＤＯ等の溶存ガスをガス透過膜を透過させ
て気室に移行させて除去するものであり、水中の溶存ガ
スを極低濃度にまで除去することができる。In such an ultrapure water production apparatus, it is required to remove DO as much as possible in order to use the produced ultrapure water as wafer cleaning water. In many cases, a deaerator is further installed in the subsystem. For example, JP-A-9-29
No. 251 describes that a DO type is reduced by providing a membrane type deaerator after the ion exchange pure water apparatus. The membrane type deaerator has an air chamber and a water chamber separated by a gas permeable membrane, flows water into the water chamber, sucks the air chamber with a vacuum pump, and gas-dissolves dissolved gas such as DO in water. The gas is permeated through the membrane and moved to the air chamber to remove the dissolved gas, and the dissolved gas in the water can be removed to an extremely low concentration.
【０００４】[0004]
【発明が解決しようとする課題】膜式脱気装置をサブシ
ステムに設けた場合、ＤＯのみならず他の溶存ガスをも
除去することになる。このため、ＤＯ低減化の目的は達
成できるが、ＤＯ以外の溶存ガス濃度も低下した超純水
となる。When a membrane deaerator is provided in a subsystem, not only DO but also other dissolved gases are removed. For this reason, although the object of DO reduction can be achieved, it becomes ultrapure water in which the concentration of dissolved gases other than DO is also reduced.
【０００５】ところで、ウエハの超音波洗浄において
は、洗浄水として用いる超純水中の溶存ガスのキャビテ
ーション効果で洗浄効果が高められている。このため、
膜式脱気装置を設けたサブシステムで製造された、溶存
ガス濃度の低下した超純水では、ウエハの超音波洗浄に
おいて、キャビテーションの発生が不足し、洗浄効果が
不十分となることがある。In the ultrasonic cleaning of wafers, the cleaning effect is enhanced by the cavitation effect of dissolved gas in ultrapure water used as cleaning water. For this reason,
Ultra-pure water with a reduced dissolved gas concentration manufactured by a subsystem equipped with a membrane deaerator may cause insufficient cavitation and insufficient cleaning effect in ultrasonic cleaning of wafers. .
【０００６】また、サブシステムに膜式脱気装置が配置
されていない装置でも、一次純水システムに脱気装置が
配置され、密閉系で一次純水がサブシステムに供給され
る系では、サブシステムで溶存ガス濃度が著しく低い超
純水が製造される場合があり、上記のような問題が発生
する。Further, even in a system in which a membrane type deaerator is not provided in a subsystem, in a system in which a deaerator is provided in a primary pure water system and primary pure water is supplied to the subsystem in a closed system, a sub-system is provided. The system may produce ultrapure water with a very low dissolved gas concentration, causing the above-described problems.
【０００７】本発明は上記従来の問題点を解決し、ＤＯ
濃度がきわめて低く、一方で適度な溶存ガス濃度を有
し、ウエハの超音波洗浄に使用した場合に、良好なキャ
ビテーション効果を得ることができる超純水を製造する
ことができる超純水製造装置を提供することを目的とす
る。The present invention solves the above-mentioned conventional problems and provides a DO
Ultrapure water production equipment capable of producing ultrapure water having an extremely low concentration, while having an appropriate dissolved gas concentration and capable of obtaining a good cavitation effect when used for ultrasonic cleaning of a wafer. The purpose is to provide.
【０００８】[0008]
【課題を解決するための手段】本発明の超純水製造装置
は、サブシステムによって純水を処理して超純水を製造
する超純水製造装置において、該サブシステムは、ガス
透過膜によって隔てられた気室及び水室を有した膜式ガ
ス溶解装置を備え、該膜式ガス溶解装置の気室に実質的
に酸素を含有しないガスを水室側圧力以上で供給すると
共に、該膜式ガス溶解装置の水室に純水を通水して、該
純水にガスを溶解させるようにしたことを特徴とする。An ultrapure water producing apparatus according to the present invention is an ultrapure water producing apparatus for producing ultrapure water by treating pure water with a subsystem, wherein the subsystem comprises a gas permeable membrane. A membrane gas dissolving apparatus having a separated gas chamber and a water chamber, wherein a gas substantially free of oxygen is supplied to the gas chamber of the membrane gas dissolving apparatus at a pressure higher than the water chamber side, and It is characterized in that pure water is passed through the water chamber of the gas dissolving apparatus to dissolve the gas in the pure water.
【０００９】本発明の超純水製造装置では、サブシステ
ムに膜式ガス溶解装置を設け、純水に酸素以外のガスを
溶解させて所望の溶存ガス濃度に調整することができ
る。このため、ＤＯを低く抑えた上で溶存ガス濃度を上
げてウエハ洗浄に好適な超純水を製造することができ
る。In the apparatus for producing ultrapure water of the present invention, a membrane gas dissolving apparatus is provided in the subsystem, and a gas other than oxygen can be dissolved in pure water to adjust the dissolved gas concentration to a desired concentration. Therefore, ultrapure water suitable for wafer cleaning can be produced by increasing the dissolved gas concentration while keeping DO low.
【００１０】本発明においては、サブシステムは、膜式
脱気装置を備え、この膜式脱気装置の後段に膜式ガス溶
解装置が配置されていることが好ましく、この場合に
は、膜式脱気装置によりＤＯを極低濃度にまで除去した
後、膜式ガス溶解装置でガスを溶解させて、目的とする
極低ＤＯ濃度で所定溶存ガス濃度の超純水を製造するこ
とができる。In the present invention, the subsystem is preferably provided with a membrane type deaerator, and a membrane type gas dissolving unit is preferably disposed downstream of the membrane type deaerator. After DO is removed to an extremely low concentration by a deaerator, the gas is dissolved by a membrane gas dissolving device, and ultrapure water having a desired extremely low DO concentration and a predetermined dissolved gas concentration can be produced.
【００１１】即ち、一次純水システムからサブシステム
に供給される純水のＤＯが１０ｍｇ／Ｌ以上である場
合、或いはサブシステムにおいてＤＯが１０ｍｇ／Ｌ以
上になる恐れがある場合、サブシステムには、特開平９
−２９２５１号公報記載のように、膜式脱気装置を配置
するのが好ましい。通常、サブシステムには紫外線酸化
装置、イオン交換純水装置が設けられることが多いが、
紫外線の過剰照射は、イオン交換純水装置でのＤＯ発生
原因となるので、サブシステムに膜式脱気装置を設ける
ことが好ましい。この場合、膜式脱気装置によりＤＯの
みならず他の溶存ガスも除去されるが、その後段に膜式
ガス溶解装置を設けることにより、超純水中の溶存ガス
濃度を所望の値に高めることができる。That is, when the DO of pure water supplied from the primary pure water system to the subsystem is 10 mg / L or more, or when there is a possibility that the DO becomes 10 mg / L or more in the subsystem, the subsystem includes , JP-A-9
As described in JP-A-29251, it is preferable to dispose a membrane deaerator. Usually, the subsystem is equipped with an ultraviolet oxidation device and an ion exchange pure water device,
Since excessive irradiation of ultraviolet rays causes DO generation in the ion exchange pure water apparatus, it is preferable to provide a membrane type deaerator in the subsystem. In this case, not only DO but also other dissolved gases are removed by the membrane deaerator, but by providing a membrane gas dissolver at a subsequent stage, the dissolved gas concentration in the ultrapure water is increased to a desired value. be able to.
【００１２】また、本発明においては、膜式ガス溶解装
置の気室に供給される、実質的に酸素を含有しないガス
の流量Ｇ（Ｎｍ３／ｈｒ）に対する、膜式ガス溶解装置
の水室に通水される純水の通水量Ｌ（ｍ３／ｈｒ）の割
合であるＬ／Ｇ比が２０以下となるように、該ガス及び
一次純水を膜式ガス溶解装置に導入することが好まし
い。Further, in the present invention, the water chamber of the membrane gas dissolving apparatus is provided with respect to the flow rate G (Nm 3 / hr) of the gas substantially free of oxygen supplied to the gas chamber of the membrane gas dissolving apparatus. The gas and primary pure water may be introduced into the membrane gas dissolving apparatus so that the L / G ratio, which is the ratio of the flow rate L (m 3 / hr) of the pure water passed through the reactor, is 20 or less. preferable.
【００１３】このような本発明の超純水製造装置では、
ウエハの超音波洗浄に好適な、ＤＯ濃度１０μｇ／Ｌ以
下で、溶存ガス濃度５ｍｇ／Ｌ以上の超純水を製造する
ことができる。In such an ultrapure water producing apparatus of the present invention,
Ultrapure water having a DO concentration of 10 μg / L or less and a dissolved gas concentration of 5 mg / L or more, which is suitable for ultrasonic cleaning of wafers, can be produced.
【００１４】[0014]
【発明の実施の形態】以下に図面を参照して本発明の超
純水製造装置の実施の形態を詳細に説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the ultrapure water production apparatus of the present invention will be described below in detail with reference to the drawings.
【００１５】図１は本発明の超純水製造装置のサブシス
テムの実施の形態を示す系統図である。FIG. 1 is a system diagram showing an embodiment of a subsystem of the ultrapure water production apparatus of the present invention.
【００１６】本発明において、サブシステムで処理する
純水は、図２に示す如く、原水（工業用水、市水、井水
等）を凝集、加圧浮上（沈殿）、濾過装置等よりなる前
処理システム１及び一次純水システム２で処理して得ら
れた純水（一次純水）である。前処理システム及び一次
純水システムの構成には特に制限はなく、一次純水シス
テムとしては、逆浸透膜分離装置、イオン交換装置、非
再生式電気脱塩装置などの脱塩装置；活性炭、合成吸着
樹脂などの吸着装置；紫外線酸化装置などの酸化装置、
膜式脱気装置、真空式脱気装置、触媒式脱気装置などの
脱気装置を任意の順で配置したものを用いることができ
る。In the present invention, as shown in FIG. 2, the pure water to be treated by the subsystem is obtained by aggregating raw water (industrial water, city water, well water, etc.), pressurized flotation (sedimentation), and filtration. Pure water (primary pure water) obtained by processing in the treatment system 1 and the primary pure water system 2. The configurations of the pretreatment system and the primary pure water system are not particularly limited, and the primary pure water system includes a desalination device such as a reverse osmosis membrane separator, an ion exchange device, and a non-regenerative electric desalination device; activated carbon; Adsorption equipment such as adsorption resin; oxidation equipment such as ultraviolet oxidation equipment,
A device in which deaerators such as a membrane deaerator, a vacuum deaerator, and a catalytic deaerator are arranged in an arbitrary order can be used.
【００１７】このような一次純水システムにより、好ま
しくは比抵抗１０ＭΩ・ｃｍ以上の純水を製造し、サブ
システムに導入する。With such a primary pure water system, pure water preferably having a specific resistance of 10 MΩ · cm or more is produced and introduced into a subsystem.
【００１８】本発明において、純水を処理して超純水を
製造するサブシステムの膜式ガス溶解装置以外の構成に
も特に制限はない。一般に、サブシステムには、サブタ
ンク、熱交換器、紫外線酸化装置、イオン交換純水装
置、膜分離装置などがこの順で設けられるが、配置順序
の変更も任意であり、更に、膜式脱気装置、逆浸透膜分
離装置、電気脱塩装置などが追加される場合もある。In the present invention, there is no particular limitation on the configuration other than the membrane gas dissolving apparatus of the subsystem for producing ultrapure water by treating pure water. Generally, a subsystem is provided with a sub-tank, a heat exchanger, an ultraviolet oxidizer, an ion-exchange pure water apparatus, a membrane separator, and the like in this order. In some cases, a device, a reverse osmosis membrane separation device, an electrodeionization device and the like are added.
【００１９】図１（ａ）に示すサブシステムは、純水を
低圧紫外線酸化装置１１、膜式ガス溶解装置１２、イオ
ン交換純水装置１３及び限外濾過膜分離装置１４で順次
処理するものである。The subsystem shown in FIG. 1A sequentially processes pure water in a low-pressure ultraviolet oxidizing apparatus 11, a membrane gas dissolving apparatus 12, an ion exchange pure water apparatus 13, and an ultrafiltration membrane separation apparatus 14. is there.
【００２０】低圧紫外線酸化装置１１としては、波長１
７０ｎｍ以上、好ましくは１８０〜２００ｎｍの紫外線
を照射して純水中のＴＯＣを分解するものであれば良
く、特に制限はない。また、イオン交換純水装置１３及
び限外濾過膜分離装置１４としても、特に制限はなく、
通常のサブシステムに用いられているものを使用するこ
とができる。The low-pressure ultraviolet oxidation device 11 has a wavelength 1
There is no particular limitation as long as it decomposes TOC in pure water by irradiating ultraviolet rays of 70 nm or more, preferably 180 to 200 nm. Also, the ion exchange pure water apparatus 13 and the ultrafiltration membrane separation apparatus 14 are not particularly limited.
What is used for a normal subsystem can be used.
【００２１】膜式ガス溶解装置１２は、その構成自体は
通常の膜式脱気装置と同様の構成とされており、ガス透
過膜を介して気室と水室とが仕切られたものである。こ
の膜式ガス溶解装置１２では、水室に低圧紫外線酸化装
置１１で処理した純水を通水すると共に、気室に、実質
的に酸素を含有しないガスを水室側圧力以上で供給する
ことにより、該ガスをガス透過膜を透過させて水側へ移
行させることにより、水の溶存ガス濃度を高める。膜式
ガス溶解装置１２の気室の圧力が水室側圧力よりも低い
と水側へのガスの移行が十分に行われないため、気室は
水室側圧力以上、好ましくは水室側圧力よりも０．０１
〜０．２ＭＰａ高い圧力、より好ましくは水室側圧力よ
りも０．０２〜０．０５ＭＰａ程度高い圧力の加圧条件
とする。The membrane gas dissolving apparatus 12 has the same structure as that of a normal membrane deaerator, and is divided into an air chamber and a water chamber via a gas permeable membrane. . In the membrane gas dissolving apparatus 12, pure water treated by the low-pressure ultraviolet oxidizing apparatus 11 is passed through the water chamber, and a gas substantially free of oxygen is supplied to the gas chamber at a pressure higher than the water chamber side pressure. Thereby, the dissolved gas concentration of water is increased by permeating the gas to the water side through the gas permeable membrane. If the pressure of the air chamber of the membrane gas dissolving device 12 is lower than the water chamber side pressure, the gas is not sufficiently transferred to the water side, so the air chamber is at or above the water chamber side pressure, preferably the water chamber side pressure. 0.01 than
The pressure is set to a pressure higher by 0.2 MPa, more preferably 0.02 to 0.05 MPa higher than the pressure on the water chamber side.
【００２２】膜式ガス溶解装置１２の気室に供給する、
実質的に酸素を含まないガスとしては、得られた超純水
をウエハの洗浄に使用した場合特に洗浄効果に影響しな
いガス、例えば、窒素（Ｎ２）、アルゴンなどの不活性
ガスや、洗浄に使用した場合、洗浄効果を向上させる有
用ガス、例えば水素、アンモニアなどが挙げられるが、
不活性ガスであれば、製造した超純水を任意の洗浄工程
に使用することができ好ましい。このガスは、酸素を含
まないことが好ましいが、得られる超純水のＤＯ濃度を
目的とする低濃度に抑えられる程度であれば、微量の酸
素を含んでいてもよい。The gas is supplied to the gas chamber of the membrane type gas dissolving apparatus 12.
As the gas substantially free of oxygen, a gas that does not particularly affect the cleaning effect when the obtained ultrapure water is used for cleaning a wafer, for example, an inert gas such as nitrogen (N 2 ) or argon, or a cleaning gas When used for, useful gas for improving the cleaning effect, such as hydrogen, ammonia and the like,
As long as it is an inert gas, the produced ultrapure water can be used for an arbitrary washing step, and thus is preferable. This gas preferably does not contain oxygen, but may contain a trace amount of oxygen as long as the DO concentration of the obtained ultrapure water can be suppressed to a target low concentration.
【００２３】膜式ガス溶解装置１２に供給するガスとし
ては、特に純度９９．９％以上のＮ ２ガスが好ましい。The gas supplied to the film-type gas dissolving apparatus 12
In particular, N with a purity of 99.9% or more 2Gas is preferred.
【００２４】この膜式ガス溶解装置１２のＬ／Ｇ比は、
２０以下、好ましくは１０〜２０とする。この範囲より
もＬ／Ｇ比が小さいと、供給ガス量が多くなり不経済で
あり、多いとガス量が不足して溶存ガス濃度を十分に高
めることができない場合がある。The L / G ratio of the membrane type gas dissolving apparatus 12 is as follows:
20 or less, preferably 10 to 20. If the L / G ratio is smaller than this range, the supply gas amount increases and it is uneconomical. If the L / G ratio is too large, the gas amount may be insufficient and the dissolved gas concentration may not be sufficiently increased.
【００２５】このような膜式ガス溶解装置１２はサブシ
ステムの任意の箇所に設けられる。図１（ａ）に示すサ
ブシステムは、低圧紫外線酸化装置１１、膜式ガス溶解
装置１２、イオン交換純水装置１３及び限外濾過膜分離
装置１４で順次処理するものであるが、図１（ｂ）に示
す如く、低圧紫外線酸化装置１１、イオン交換純水装置
１３、膜式ガス溶解装置１２及び限外濾過膜分離装置１
４で順次処理するものであっても良い。ただし、膜式ガ
ス溶解装置１２の後段にイオン交換純水装置１３を設け
た場合には、膜式ガス溶解装置１２から溶出した微量イ
オンをイオン交換純水装置１３で除去することができ、
好ましい。Such a film-type gas dissolving apparatus 12 is provided at an arbitrary position in a subsystem. The subsystem shown in FIG. 1 (a) sequentially processes the low-pressure ultraviolet oxidation device 11, the membrane gas dissolving device 12, the ion exchange pure water device 13, and the ultrafiltration membrane separation device 14. As shown in b), a low-pressure ultraviolet oxidation apparatus 11, an ion exchange pure water apparatus 13, a membrane gas dissolving apparatus 12, and an ultrafiltration membrane separation apparatus 1
4 may be sequentially processed. However, when the ion exchange pure water device 13 is provided at the subsequent stage of the membrane gas dissolution device 12, trace ions eluted from the membrane gas dissolution device 12 can be removed by the ion exchange pure water device 13.
preferable.
【００２６】また、前述の如く、サブシステムに膜式脱
気装置を設ける場合があるが、この場合には、膜式ガス
溶解装置は膜式脱気装置の後段に設ける。図１（ｃ）
は、膜式脱気装置１５を設けたサブシステムの例を示
し、このサブシステムでは、純水は、低圧紫外線酸化装
置１１、膜式脱気装置１５、膜式ガス溶解装置１２、イ
オン交換純水装置１３及び限外濾過膜分離装置１４で順
次処理される。この場合にも、膜式脱気装置１５及び膜
式ガス溶解装置１２の後段にイオン交換純水装置１３が
設けられているため、膜式脱気装置１５及び膜式ガス溶
解装置１２から溶出した微量イオンをイオン交換純水装
置１３で除去することができ好ましい。As described above, the subsystem may be provided with a membrane deaerator, but in this case, the membrane gas dissolving apparatus is provided after the membrane deaerator. FIG. 1 (c)
Shows an example of a subsystem provided with a membrane deaerator 15, in which the pure water is supplied from a low-pressure ultraviolet oxidizer 11, a membrane deaerator 15, a membrane gas dissolver 12, an ion exchange The water is sequentially processed in the water device 13 and the ultrafiltration membrane separation device 14. Also in this case, since the ion exchange pure water apparatus 13 is provided at the subsequent stage of the membrane type deaerator 15 and the membrane type gas dissolving apparatus 12, the eluted from the membrane type deaerator 15 and the membrane type gas dissolving apparatus 12. Trace ions can be preferably removed by the ion-exchange pure water apparatus 13.
【００２７】膜式脱気装置１５は、膜式ガス溶解装置１
２と同様にガス透過膜を介して気室と水室とが仕切られ
たものであり、この膜式脱気装置１５では、水室に低圧
紫外線酸化装置１１で処理した純水を通水すると共に、
気室を真空ポンプ（図示せず）により２０〜１００Ｔｏ
ｒｒ（２．７×１０−３〜１．３×１０−２ＭＰａ）程
度の真空度に吸引して、水中のＤＯ等の溶存ガスをガス
透過膜を透過させて気室側に移行させて除去する。The membrane deaerator 15 is a membrane gas dissolver 1
The air chamber and the water chamber are separated through a gas permeable membrane in the same manner as in 2, and in this membrane deaerator 15, pure water treated by the low-pressure ultraviolet oxidation device 11 is passed through the water chamber. Along with
The air chamber is evacuated by a vacuum pump (not shown) to 20-100 To.
Suction is performed to a degree of vacuum of about rr (2.7 × 10 −3 to 1.3 × 10 −2 MPa), and dissolved gas such as DO in water passes through the gas permeable membrane and is transferred to the air chamber side. Remove.
【００２８】この膜式脱気装置１５の気室には、必要に
応じて、Ｎ２、アルゴン等の不活性ガスを供給しても良
い。膜式脱気装置１５の気室にガスを供給することによ
り、脱気効率を高めることができる。この場合、不活性
ガスの供給量は、多過ぎると気室の真空度が上がらず、
少な過ぎると脱気効率の向上効果を十分に得ることがで
きないことから、Ｌ／Ｇ比で２０〜４０程度とするのが
好ましい。An inert gas such as N 2 or argon may be supplied to the air chamber of the membrane deaerator 15 as necessary. By supplying gas to the air chamber of the membrane type deaerator 15, the deaeration efficiency can be increased. In this case, if the supply amount of the inert gas is too large, the degree of vacuum in the air chamber does not increase,
If the amount is too small, the effect of improving the deaeration efficiency cannot be sufficiently obtained, so that the L / G ratio is preferably about 20 to 40.
【００２９】なお、本発明において、膜式ガス溶解装置
及び膜式脱気装置に用いられるガス透過膜としては、Ｏ
２，Ｎ２等のガスは通過するが水は透過しない膜であれ
ば良く、例えば、ポリプロピレン系、シリコンゴム系、
ポリテトラフルオロエチレン系、ポリオレフィン系、ポ
リウレタン系等がある。また、膜形式についても特に制
限はなく、中空糸、スパイラル型等の各種のものを用い
ることができるが、特に中空糸型が好適である。このガ
ス透過膜としては市販の各種のものを用いることができ
る。In the present invention, the gas permeable membrane used in the membrane gas dissolving apparatus and the membrane deaerator is O
2, the gas such as N 2 is passed may be a film that water does not pass through, for example, polypropylene, silicone rubber,
Examples include polytetrafluoroethylene, polyolefin, and polyurethane. The type of the membrane is not particularly limited, and various types such as a hollow fiber and a spiral type can be used. The hollow fiber type is particularly preferable. Various commercially available gas permeable membranes can be used.
【００３０】本発明において、ウエハの超音波洗浄水の
用途においては、このようなサブシステムにより、ＤＯ
１００ｐｐｂ以下、Ｎ２等のＤＯ以外の溶存ガス濃度５
ｍｇ／Ｌ以上、好ましくはＤＯが１０ｐｐｂ以下で溶存
ガス濃度が５〜１２ｍｇ／Ｌ程度の超純水を製造するこ
とが好ましい。In the present invention, in the use of ultrasonic cleaning water for wafers, DO
100ppb or less, the dissolved gas concentration of the non-DO etc. N 2 5
It is preferable to produce ultrapure water of not less than mg / L, preferably not more than 10 ppb and having a dissolved gas concentration of about 5 to 12 mg / L.
【００３１】[0031]
【実施例】以下に実施例及び比較例を挙げて本発明をよ
り具体的に説明する。The present invention will be described more specifically below with reference to examples and comparative examples.
【００３２】実施例１ 市水（電導度：１．１ｍｓ／ｍ，ＤＯ濃度：７．２ｍｇ
／Ｌ，Ｎ２（溶解Ｎ２）濃度：１２．１ｍｇ／Ｌ）を逆
浸透膜分離装置、混床式イオン交換純水装置及び膜式脱
気装置で順次処理して得られた、比抵抗１７ＭΩ・ｃ
ｍ，ＤＯ濃度：１００μｇ／Ｌ，Ｎ２濃度：２．５ｍｇ
／Ｌの純水を図１（ｃ）に示すサブシステムに１．５ｍ
３／ｈｒで通水して処理する超純水製造装置において、
膜式ガス溶解装置によるガス溶解効果を調べた。Example 1 City water (conductivity: 1.1 ms / m, DO concentration: 7.2 mg)
/ L, N 2 (dissolved N 2 ) concentration: 12.1 mg / L) were sequentially processed by a reverse osmosis membrane separator, a mixed bed type ion exchange pure water system and a membrane type deaerator, and the specific resistance was obtained. 17MΩ ・ c
m, DO concentration: 100 μg / L, N 2 concentration: 2.5 mg
/ L of pure water 1.5 m into the subsystem shown in FIG.
In an ultrapure water production apparatus that treats by passing water at 3 / hr,
The effect of gas dissolution by a membrane gas dissolution apparatus was investigated.
【００３３】低圧紫外線酸化装置（日本フォトサイエン
ス（株）製；ＯＸＬ型ランプ４本）１１に通水した後の
純水を膜式脱気装置（セルガード社製、４インチガス透
過膜）１５に通水した後膜式ガス溶解装置（セルガード
社製、４インチガス透過膜）１２に通水した。Pure water after passing water through a low-pressure ultraviolet oxidation device (manufactured by Japan Photo Science Co., Ltd .; four OXL-type lamps) 11 is passed to a membrane type deaerator (4-inch gas permeable membrane manufactured by Celgard) 15. After passing water, water was passed through a membrane-type gas dissolution apparatus (Celgard, 4 inch gas permeable membrane) 12.
【００３４】膜式脱気装置１５の気室にはＮ２ガスを
０．０５Ｎｍ３／ｈｒ（Ｌ／Ｇ比＝３０）で供給すると
共に、真空ポンプで６０Ｔｏｒｒ（８．０×１０−３Ｍ
Ｐａ）の真空度に減圧した。N 2 gas is supplied to the air chamber of the membrane deaerator 15 at 0.05 Nm 3 / hr (L / G ratio = 30), and 60 Torr (8.0 × 10 −3 M) is supplied by a vacuum pump.
The pressure was reduced to Pa).
【００３５】また、膜式ガス溶解装置１２の気室には水
室側と同圧力（大気圧よりも０．０１ＭＰａ高い圧力）
でＮ２を０．０７５Ｎｍ３／ｈｒで供給した（Ｌ／Ｇ比
＝２０）。The pressure in the gas chamber of the membrane gas dissolving apparatus 12 is the same as that of the water chamber (pressure higher than the atmospheric pressure by 0.01 MPa).
And N 2 was supplied at 0.075 Nm 3 / hr (L / G ratio = 20).
【００３６】得られた超純水のＤＯ濃度とＮ２濃度を調
べ、結果を表１に示した。The DO concentration and N 2 concentration of the obtained ultrapure water were examined, and the results are shown in Table 1.
【００３７】実施例２ 実施例１において、膜式ガス溶解装置１２の気室の圧力
を水室側よりも０．０５ＭＰａ高い条件としたこと以外
は同様にして処理を行い、得られた超純水のＤＯ濃度と
Ｎ２濃度を調べ、結果を表１に示した。Example 2 The procedure of Example 1 was repeated, except that the pressure in the gas chamber of the membrane-type gas dissolving apparatus 12 was set to 0.05 MPa higher than that in the water chamber side. examine the DO concentration and the N 2 concentration of water, the results are shown in Table 1.
【００３８】比較例１ 実施例１において、膜式ガス溶解装置１２の代りに膜式
脱気装置（セルガード社製、４インチガス透過膜）を設
けて、２段膜脱気を行ったこと以外は同様にして処理を
行い、得られた超純水のＤＯ濃度とＮ２濃度を調べ、結
果を表１に示した。Comparative Example 1 In Example 1, a two-stage membrane deaeration was performed by providing a membrane deaerator (4 inch gas permeable membrane, manufactured by Celgard) instead of the membrane gas dissolver 12. performs processing in the same manner to examine the dO concentration and the concentration of N 2 ultrapure water obtained results are shown in Table 1.
【００３９】なお、この２段目の膜式脱気装置も１段目
の膜式脱気装置と同様に、気室にＮ ２ガスを０．０５Ｎ
ｍ３／ｈｒで供給すると共に、真空ポンプで６０Ｔｏｒ
ｒに減圧した。The second-stage membrane deaerator is also a first-stage membrane deaerator.
As in the case of the membrane deaerator of 20.05N gas
m3/ Hr and 60 Torr by vacuum pump
The pressure was reduced to r.
【００４０】[0040]
【表１】 [Table 1]
【００４１】表１より明らかなように、本発明によれ
ば、ＤＯ濃度がきわめて低く、Ｎ２濃度が適度に高い超
純水を製造することができる。As is apparent from Table 1, according to the present invention, DO concentration is very low, it is possible to N 2 concentration to produce a reasonably high ultrapure water.
【００４２】[0042]
【発明の効果】以上詳述した通り、本発明の超純水製造
装置によれば、ＤＯ濃度が著しく低く、かつ十分な溶存
ガス濃度の超純水を製造することができる。本発明の超
純水製造装置により製造された超純水は、ウエハの超音
波洗浄水として、良好なキャビテーション効果で高い洗
浄効果を得ることができる。As described in detail above, according to the apparatus for producing ultrapure water of the present invention, ultrapure water having an extremely low DO concentration and a sufficient dissolved gas concentration can be produced. The ultrapure water produced by the ultrapure water production apparatus of the present invention can provide a high cavitation effect and a high cleaning effect as ultrasonic cleaning water for wafers.
【図１】本発明の超純水製造装置のサブシステムの実施
の形態を示す系統図である。FIG. 1 is a system diagram showing an embodiment of a subsystem of an ultrapure water production apparatus of the present invention.
【図２】従来の超純水製造装置を示す系統図である。FIG. 2 is a system diagram showing a conventional ultrapure water production apparatus.
１ 前処理システム ２ 一次純水システム ３ サブシステム １１ 低圧紫外線酸化装置 １２ 膜式ガス溶解装置 １３ イオン交換純水装置 １４ 限外濾過膜分離装置 １５ 膜式脱気装置 DESCRIPTION OF SYMBOLS 1 Pretreatment system 2 Primary pure water system 3 Subsystem 11 Low-pressure ultraviolet oxidation apparatus 12 Membrane gas dissolving apparatus 13 Ion exchange pure water apparatus 14 Ultrafiltration membrane separation apparatus 15 Membrane deaerator
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ０２Ｆ 1/68 Ｃ０２Ｆ 1/68 ５４０Ｃ ５４０Ｄ ５４０Ｚ Ｂ０１Ｄ 19/00 Ｂ０１Ｄ 19/00 Ｈ Ｂ０１Ｆ 1/00 Ｂ０１Ｆ 1/00 Ａ 5/06 5/06 Ｃ０２Ｆ 1/20 Ｃ０２Ｆ 1/20 Ａ // Ｂ０１Ｄ 61/00 Ｂ０１Ｄ 61/00 Ｃ０２Ｆ 1/44 Ｃ０２Ｆ 1/44 Ｊ Ｆターム(参考） 4D006 GA06 JA51 JA66 JA67 KA53 KA57 KE02 KE06 KE13Q PB06 PB62 PB63 PC02 4D011 AA16 AD00 4D037 AA03 AB11 BA23 CA03 4G035 AA01 AE13 AE17 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C02F 1/68 C02F 1/68 540C 540D 540Z B01D 19/00 B01D 19/00 H B01F 1/00 B01F 1 / 00 A 5/06 5/06 C02F 1/20 C02F 1/20 A // B01D 61/00 B01D 61/00 C02F 1/44 C02F 1/44 J F term (reference) 4D006 GA06 JA51 JA66 JA67 KA53 KA57 KE02 KE06 KE13Q PB06 PB62 PB63 PC02 4D011 AA16 AD00 4D037 AA03 AB11 BA23 CA03 4G035 AA01 AE13 AE17
Claims (4)
純水を製造する超純水製造装置において、 該サブシステムは、ガス透過膜によって隔てられた気室
及び水室を有した膜式ガス溶解装置を備え、 該膜式ガス溶解装置の気室に実質的に酸素を含有しない
ガスを水室側圧力以上で供給すると共に、該膜式ガス溶
解装置の水室に純水を通水して、該純水にガスを溶解さ
せるようにしたことを特徴とする超純水製造装置。1. An ultrapure water producing apparatus for producing ultrapure water by treating pure water with a subsystem, the subsystem comprising a membrane gas having an air chamber and a water chamber separated by a gas permeable membrane. A gas dissolving device, a gas containing substantially no oxygen is supplied to the gas chamber of the membrane gas dissolving device at a pressure higher than the water chamber side pressure, and pure water is passed through the water chamber of the membrane gas dissolving device. An ultrapure water producing apparatus, wherein a gas is dissolved in the pure water.
膜式脱気装置を備えており、該膜式脱気装置の後段に前
記膜式ガス溶解装置が配置されていることを特徴とする
超純水製造装置。2. The system of claim 1, wherein the subsystem comprises:
An ultrapure water production apparatus, comprising a membrane deaerator, wherein the membrane gas dissolving apparatus is arranged at a stage subsequent to the membrane deaerator.
解装置の気室に供給される、前記実質的に酸素を含有し
ないガスの流量（Ｎｍ３／ｈｒ）に対する、該膜式ガス
溶解装置の水室に通水される純水の通水量（ｍ３／ｈ
ｒ）の割合であるＬ／Ｇ比が２０以下となるように、該
ガス及び純水が該膜式ガス溶解装置に導入されることを
特徴とする超純水製造装置。3. The film-type gas dissolving device according to claim 1, wherein a flow rate (Nm 3 / hr) of the substantially oxygen-free gas supplied to an air chamber of the film-type gas dissolving device is provided. Pure water flow through the water chamber of the device (m 3 / h
The ultrapure water production apparatus, wherein the gas and pure water are introduced into the membrane gas dissolving apparatus so that the L / G ratio, which is the ratio of r), is 20 or less.
て、溶存酸素濃度１０μｇ／Ｌ以下で、溶存ガス濃度５
ｍｇ／Ｌ以上の超純水を製造することを特徴とする超純
水製造装置。4. The method according to claim 1, wherein the dissolved oxygen concentration is not more than 10 μg / L and the dissolved gas concentration is not more than 10 μg / L.
An ultrapure water production apparatus for producing ultrapure water of not less than mg / L.
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|---|---|---|---|
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| WO2018055801A1 (en) * | 2016-09-20 | 2018-03-29 | 栗田工業株式会社 | Dilute chemical solution-producing apparatus and dilute chemical solution-producing method |
| JP2018049872A (en) * | 2016-09-20 | 2018-03-29 | 栗田工業株式会社 | Diluted chemical manufacturing apparatus and diluted chemical manufacturing method |
| KR20190053816A (en) * | 2016-09-20 | 2019-05-20 | 쿠리타 고교 가부시키가이샤 | Diluent liquid manufacturing apparatus and diluting liquid manufacturing method |
| US10759678B2 (en) | 2016-09-20 | 2020-09-01 | Kurita Water Industries Ltd. | Dilute chemical solution producing apparatus and dilute chemical solution producing method |
| TWI746528B (en) * | 2016-09-20 | 2021-11-21 | 日商栗田工業股份有限公司 | Diluted medicinal solution manufacturing device and diluted medicinal solution manufacturing method |
| KR102429860B1 (en) * | 2016-09-20 | 2022-08-04 | 쿠리타 고교 가부시키가이샤 | Diluted chemical solution manufacturing apparatus and diluted chemical solution manufacturing method |
| CN111573781A (en) * | 2017-05-18 | 2020-08-25 | 三菱重工环境·化学工程株式会社 | Biological treatment method |
| US12486187B2 (en) | 2022-04-18 | 2025-12-02 | Disco Corporation | Wafer production system and wafer manufacturing method |
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