JPH10272492A - High-temperature ultrapure water production apparatus and chemical liquid preparation apparatus equipped with the same - Google Patents

High-temperature ultrapure water production apparatus and chemical liquid preparation apparatus equipped with the same

Info

Publication number
JPH10272492A
JPH10272492A JP9079277A JP7927797A JPH10272492A JP H10272492 A JPH10272492 A JP H10272492A JP 9079277 A JP9079277 A JP 9079277A JP 7927797 A JP7927797 A JP 7927797A JP H10272492 A JPH10272492 A JP H10272492A
Authority
JP
Japan
Prior art keywords
ultrapure water
temperature
water
temperature ultrapure
ion exchange
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.)
Pending
Application number
JP9079277A
Other languages
Japanese (ja)
Inventor
Koji Ban
功二 伴
Kazunori Koba
和則 木場
Shoichi Momose
祥一 百瀬
Toshinori Iwai
俊憲 岩井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Electric Corp
Kanadevia Corp
Original Assignee
Hitachi Zosen Corp
Mitsubishi Electric Corp
Hitachi Shipbuilding and Engineering Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hitachi Zosen Corp, Mitsubishi Electric Corp, Hitachi Shipbuilding and Engineering Co Ltd filed Critical Hitachi Zosen Corp
Priority to JP9079277A priority Critical patent/JPH10272492A/en
Priority to CNB988112922A priority patent/CN1163418C/en
Priority to PCT/JP1998/004214 priority patent/WO2000017108A1/en
Priority to US09/554,558 priority patent/US6562205B1/en
Priority to TW087115916A priority patent/TW514626B/en
Publication of JPH10272492A publication Critical patent/JPH10272492A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/06Flash distillation
    • B01D3/065Multiple-effect flash distillation (more than two traps)
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/045Treatment of water, waste water, or sewage by heating by distillation or evaporation for obtaining ultra-pure water
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/20Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/441Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/4618Devices therefor; Their operating or servicing for producing "ionised" acidic or basic water
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • C02F2001/425Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • C02F2001/427Treatment of water, waste water, or sewage by ion-exchange using mixed beds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/02Non-contaminated water, e.g. for industrial water supply
    • C02F2103/04Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/346Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from semiconductor processing, e.g. waste water from polishing of wafers

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a high-temp. ultrapure water producing apparatus which does not require a metal ion elution preventive treatment and a chemical liquid preparing apparatus equipped therewith. SOLUTION: This high-temp. ultrapure water producing apparatus consists of an evaporator 22 which yields the ultrapure water of a high temp. by treating the pretreated water obtd. by a pretreating system or the primary pure water obtd. by a primary pure water system 21, an ion exchange device 23 which removes the trace metal ions included in the ultrapure water obtd. by the evaporator 22, a produced water heat exchanger 24 which is made of titanium and subjects the high-temp. ultrapure water not yet removed of the trace metal ions obtd. by the evaporator 22 and the ordinary-temp. ultrapure water subjected to the removal of the trace metal ions treated in the ion exchange device 23 to a heat exchange and a cooling heat exchanger 25 which is made of SUS, cools the ultrapure water not removed of the trace metal ions cooled by the produced water heat exchanger 24 down to <=40 deg.C and supplies the water as the supply water to the ion exchange device 23. The ultrapure water subjected to the removal of the trace metal ions heated to the high temp. by the produced water heat exchanger 24 is made into electrolytic ion water by the chemical liquid preparing apparatus or is mixed with chemicals, and is used in the treating stage of a semiconductor production process.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】この発明は、半導体工業等の
電子工業で使用される超純水製造装置に関し、特に、半
導体製造工程でのウエハ洗浄においてリンス効率および
乾燥効率の向上に顕著な効果を示す高温の超純水を得る
高温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 ultrapure water production apparatus used in the electronics industry such as the semiconductor industry, and more particularly, to a remarkable effect of improving rinsing efficiency and drying efficiency in wafer cleaning in a semiconductor manufacturing process. The present invention relates to a high-temperature ultrapure water production apparatus for obtaining the high-temperature ultrapure water shown.

【0002】また、半導体もしくはその他の精密デバイ
スの処理工程、特に半導体ウエハの洗浄等で用いられる
薬液の調製装置に関し、特に、高温の薬液を調整・供給
するさいに用いられる薬液調製装置に関する。
[0002] The present invention also relates to an apparatus for preparing a chemical solution used in a process of processing semiconductors or other precision devices, particularly for cleaning semiconductor wafers, and more particularly to an apparatus for preparing and supplying a high-temperature chemical solution.

【0003】なお、この明細書において、「薬液」と
は、半導体ウエハの洗浄工程やその他の精密デバイスの
洗浄工程で用いられる洗浄液のほか、半導体の処理工程
においてSi表面の自然酸化膜抑制用などに用いられる
プロセス液も含むものとする。
[0003] In this specification, the term "chemical solution" refers to a cleaning solution used in a semiconductor wafer cleaning process and a cleaning process for other precision devices, and also for suppressing a natural oxide film on a Si surface in a semiconductor processing process. It also includes the process liquid used in the process.

【0004】[0004]

【従来の技術】近年、半導体工業等の電子工業では、極
めて高度に精製された水が必要とされている。この精製
水の原水としては、通常、工業用水、上水道水、井戸水
等が用いられているが、これら原水中には懸濁物質、電
解質、微粒子、微生物、有機物、溶存酸素等が、要求さ
れる水質基準値を大きく越えた量で含まれているため、
これら不純物を除去しなければならない。
2. Description of the Related Art In recent years, the electronics industry, such as the semiconductor industry, requires highly purified water. As the raw water of the purified water, industrial water, tap water, well water and the like are usually used, and in these raw waters, suspended substances, electrolytes, fine particles, microorganisms, organic substances, dissolved oxygen, and the like are required. Because it is contained in an amount that greatly exceeds the water quality standard value,
These impurities must be removed.

【0005】従来、上記の如き不純物を除去して超純水
を得る装置としては、図3に示すものおよび図4に示す
ものが知られている。
Conventionally, as an apparatus for obtaining ultrapure water by removing impurities as described above, those shown in FIGS. 3 and 4 are known.

【0006】図3に示す従来例1の装置(71)は、原水を
処理する一次純水系(72)と、一次純水系(72)で得られた
一次純水を処理して超純水を得る2次純水系(73)とより
なる。一次純水系(72)は、濾過装置(74)、逆浸透装置(7
5)、脱気装置(76)およびイオン交換装置(77)よりなり、
2次純水系(73)は、紫外線殺菌装置(78)、デミネライザ
ー(79)および限外濾過(UF)装置(80)よりなる。この
装置(71)によると、供給原水中のイオン成分は、逆浸透
装置(75)、イオン交換装置(77)、デミネライザー(79)に
より極めて微量となるまで除去され、例えば抵抗率1
8.0MΩ・cm以上の超純水を得ることができる。し
かしながら、この装置(71)には、シリカや有機物などの
非イオン性不純物の除去性能が不十分であること、生産
水中の溶存酸素を充分下げることが困難であること、装
置(71)が常温下で操作されるためバクテリアの発生・増
殖が避けられず装置を停止して殺菌処理することが必要
であること、多数の処理装置を組み合わせるため、装置
(71)の構成が複雑となると共に、運転監視が面倒なもの
となることなどの問題があった。
[0006] An apparatus (71) of prior art example 1 shown in Fig. 3 comprises a primary pure water system (72) for treating raw water, and a primary pure water obtained by the primary pure water system (72) for treating ultrapure water. The obtained secondary pure water system (73). The primary pure water system (72) consists of a filtration device (74) and a reverse osmosis device (7
5), consisting of a degasser (76) and an ion exchanger (77),
The secondary pure water system (73) includes an ultraviolet sterilizer (78), a demineralizer (79), and an ultrafiltration (UF) device (80). According to this device (71), ionic components in the feed water are removed to a very small amount by a reverse osmosis device (75), an ion exchange device (77), and a demineralizer (79).
Ultrapure water of 8.0 MΩ · cm or more can be obtained. However, this device (71) has an insufficient performance of removing nonionic impurities such as silica and organic substances, it is difficult to sufficiently reduce dissolved oxygen in production water, and the device (71) has Because it is operated below, it is inevitable that bacteria generation and proliferation are inevitable and it is necessary to stop the device and sterilize it.
There are problems that the configuration of (71) becomes complicated and that operation monitoring becomes troublesome.

【0007】他方、図4に示す従来例2の装置は、従来
例1の装置では十分に除去できなかったシリカや有機物
コロイドなどの非イオン性の不純物および溶存酸素を完
全に除去し、しかも、リンス効率および乾燥効率を向上
させるのに適した温度の高温超純水を製造することを企
図したものである。
On the other hand, the apparatus of the prior art 2 shown in FIG. 4 completely removes nonionic impurities such as silica and organic colloids and dissolved oxygen which could not be sufficiently removed by the apparatus of the conventional example 1, and furthermore, It is intended to produce high-temperature ultrapure water at a temperature suitable for improving rinsing efficiency and drying efficiency.

【0008】従来例2の装置は、一次純水系で得られた
一次純水を処理して高温超純水を得る多重効用蒸発器
(I) を主体とし、その後流に限外濾過(UF)装置(2)
を備えたものである。一次純水系は、従来例1の装置に
おける一次純水系と同じものである。蒸発器(I) に供給
された一次純水は、蒸発器(I) 内の各効用段を縦貫する
予熱管(5) に導かれ、各効用段の蒸発管(7) 内で発生し
た水蒸気の一部の凝縮潜熱を受けて加熱され、第1効用
段内の予熱管(5) で加熱蒸気の一部の凝縮潜熱を受けて
100℃程度の所定温度に加熱され、第1効用段底部の
水溜部(13)に入る。水溜部(13)に入った供給水は蒸発管
(7) 内で水蒸気を発生した残りの濃縮液と混合し、混合
液の大部分は循環ポンプ(6) を介して第1効用段上部に
配置された蒸発管(7) 内を薄膜状に流下し、管外面から
加熱蒸気の大半の凝縮潜熱を受けて100℃程度の温度
で蒸発し水蒸気を発生する。水蒸気を発生した濃縮液は
水溜部(13)に流下し、前記の如く供給水と混合し、その
大半は循環ポンプ(6) を介して上部水室(15)に送られ
る。残りの混合液は連通口(14)を通って第2効用段水溜
部に入り、ここで同じく蒸発管内から流下する濃縮液と
混合し、その大部分は第2効用段の循環ポンプを介して
第2効用段上部水室に送られる。
[0008] The apparatus of the prior art 2 is a multiple effect evaporator for obtaining high-temperature ultrapure water by treating primary pure water obtained in a primary pure water system.
Ultrafiltration (UF) equipment mainly consisting of (I) and downstream (2)
It is provided with. The primary pure water system is the same as the primary pure water system in the device of Conventional Example 1. The primary pure water supplied to the evaporator (I) is led to the preheating pipe (5) that runs through each effect stage in the evaporator (I), and the steam generated in the evaporator tube (7) of each effect stage Is heated by receiving a part of the latent heat of condensation, and is heated to a predetermined temperature of about 100 ° C. by receiving a part of the latent heat of condensation of the heated steam in the preheating pipe (5) in the first effect stage. Into the water reservoir (13). The supply water entering the sump (13) is
(7) is mixed with the remaining concentrated liquid that has generated steam, and most of the mixed liquid is formed into a thin film through the circulation pump (6) in the evaporating pipe (7) arranged above the first effect stage. It flows down and receives most of the latent heat of condensation of the heated steam from the outer surface of the tube to evaporate at a temperature of about 100 ° C. to generate steam. The concentrated liquid having generated the steam flows down to the water reservoir (13), mixes with the supply water as described above, and most of the water is sent to the upper water chamber (15) via the circulation pump (6). The remaining liquid mixture enters the second effect stage reservoir through the communication port (14), where it is mixed with the concentrated liquid also flowing down from the evaporating tube, most of which is passed through the second effect stage circulation pump. It is sent to the water chamber above the second utility stage.

【0009】第1効用段の蒸発管で発生した水蒸気は、
ミスト分離器(16)を経て第2効用段内の蒸発管外部に入
る。水蒸気に同伴するミストは、ミスト分離器(16)によ
り除去されて極めて微量となる。この水蒸気の大部分は
蒸発管外面で凝縮し、凝縮液は第2効用段内の凝縮液収
集部(図示省略)に入り、残余の水蒸気は第2効用段予
熱管外面で凝縮し、凝縮液は凝縮液収集部で蒸発管から
の凝縮液と混合し、その全部が第3効用段内の凝縮液収
集部に入る。
[0009] The water vapor generated in the evaporator tube of the first effect stage is
After passing through the mist separator (16), it enters the outside of the evaporation tube in the second effect stage. The mist accompanying the water vapor is removed by the mist separator (16) and becomes extremely small. Most of the water vapor condenses on the outer surface of the evaporator tube, the condensate enters a condensate collector (not shown) in the second effect stage, and the remaining water vapor condenses on the outer surface of the preheater tube of the second effect stage. Is mixed with the condensate from the evaporating tube in the condensate collection part, and all of it enters the condensate collection part in the third effect stage.

【0010】こうして各効用段において上記プロセスが
繰り返される。
Thus, the above process is repeated at each effect stage.

【0011】最終効用段(第n効用段)で蒸発して生じ
た水蒸気は、ミスト分離器を経由して、最終効用段に近
接した復水器(1) の凝縮管(12)外面で凝縮し、凝縮液は
復水器下部の水溜部(11)に入る。また、各効用段内で凝
縮した全ての凝縮液は、凝縮液収集部を通ってやはり水
溜部(11)に入る。水溜部(11)に溜まった凝縮液は、超純
水ポンプ(10)で抜き出され、微粒子除去を目的とした限
外濾過装置(2) に通水される。
The water vapor generated by evaporation in the final effect stage (n-th effect stage) passes through a mist separator and condenses on the outer surface of the condenser tube (12) of the condenser (1) close to the final effect stage. Then, the condensate enters the water reservoir (11) at the bottom of the condenser. Also, all the condensate condensed in each effect stage also passes through the condensate collection part and enters the water reservoir (11). The condensate collected in the water reservoir (11) is extracted by an ultrapure water pump (10) and passed through an ultrafiltration device (2) for removing fine particles.

【0012】超純水ポンプ(10)で抜き出され、限外濾過
膜(2) で微粒子が除去された凝縮液は、理論純水の抵抗
率に極めて近い抵抗率18.0MΩ・cm(高温の純水
を25℃に冷却して測定した値、この明細書において、
抵抗率は、すべて25℃での測定値とする)以上を有
し、TOC値および溶存酸素濃度が極めて低くかつ高温
の超純水である。半導体製造工程でのウエハ洗浄におい
てリンス効率および乾燥効率の向上に対して顕著な効果
を示す高温超純水としては、温度70〜80℃程度の高
温超純水が特に好ましい。
The condensate extracted by the ultrapure water pump (10) and having the fine particles removed by the ultrafiltration membrane (2) has a resistivity very close to the resistivity of theoretical pure water of 18.0 MΩ · cm (high temperature). Of pure water cooled to 25 ° C., and in this specification,
All the resistivity values are measured at 25 ° C.) or higher, and the ultrapure water has a very low TOC value and dissolved oxygen concentration and a high temperature. High-temperature ultrapure water having a temperature of about 70 to 80 ° C. is particularly preferable as the high-temperature ultrapure water which has a remarkable effect on the improvement of the rinsing efficiency and the drying efficiency in the wafer cleaning in the semiconductor manufacturing process.

【0013】また、半導体製造工程でのウエハ洗浄では
図5に示すように、多くの薬液が高温で使用されてい
る。これらの薬液は、ある一定枚数のウエハが処理され
ると薬液が洗浄槽より抜き出され、空の洗浄槽に新しい
薬液が所定量供給されるバッチ方式で交換されている。
Further, in the wafer cleaning in the semiconductor manufacturing process, as shown in FIG. 5, many chemicals are used at a high temperature. When a certain number of wafers are processed, the chemicals are extracted from the cleaning tank, and the chemicals are replaced by a batch method in which a predetermined amount of a new chemical is supplied to an empty cleaning tank.

【0014】従来の薬液の調整・供給は、従来例1の装
置で製造される超純水と薬液原液を各々直接洗浄槽へ所
定量供給し、所定温度になるように電気ヒーターで加温
する、あるいは、薬液調整槽に従来例1の装置で製造さ
れる超純水と薬液原液を所定量供給し、所定温度になる
ように電気ヒーターで予熱して予め調整しておき、必要
なときに薬液調整槽から洗浄槽へ供給するといった方法
である。薬液原液の自動供給装置の供給法としては、窒
素ガスによる圧送方式とポンプによる方法とがある。
In the conventional adjustment and supply of a chemical solution, ultrapure water and an undiluted chemical solution produced by the apparatus of the conventional example 1 are respectively supplied directly to a cleaning tank by a predetermined amount, and heated by an electric heater to a predetermined temperature. Alternatively, a predetermined amount of the ultrapure water and the undiluted chemical solution produced by the apparatus of Conventional Example 1 is supplied to the chemical solution adjusting tank, and preheated with an electric heater so as to reach a predetermined temperature, and adjusted in advance. It is a method of supplying from a chemical solution adjusting tank to a washing tank. As a supply method of the automatic supply device for a drug solution, there are a pumping method using nitrogen gas and a method using a pump.

【0015】[0015]

【発明が解決しようとする課題】上記の従来例2の高温
超純水装置では、熱交換のための熱伝達率を良くするた
め蒸発管等の装置構成材料はSUS316、SUS30
4等の金属材料とされている。そして、これら金属材料
に含まれる金属イオンが凝縮液に溶出するのを防ぐため
に、接液部分を電解複合研磨して高温炉で処理し、構成
材料表面に積極的に酸化皮膜を作るといった処理が行な
われている。従来例2の装置は、このような処理を必要
とするため、装置製作の工程が複雑であり、装置製造コ
ストが高いといった問題があった。
In the high-temperature ultrapure water apparatus of the prior art 2 described above, in order to improve the heat transfer coefficient for heat exchange, the constituent materials of the apparatus such as the evaporating tube are SUS316 and SUS30.
4 and the like. In order to prevent metal ions contained in these metal materials from being eluted into the condensate, the wetted part is electrolytically polished and treated in a high-temperature furnace to form an oxide film on the surface of the constituent materials. Is being done. The device of the conventional example 2 requires such processing, so that the process of manufacturing the device is complicated, and there is a problem that the device manufacturing cost is high.

【0016】なお、従来例2の高温超純水装置におい
て、上記溶出防止処理を実施しない場合、得られた高温
超純水には、Fe50ppt、Ni10ppt程度の金
属イオンが含まれることが確認されている。半導体製造
工程では、ウエハ表面に金属イオンが1×1010ato
ms/cm2 以上あることは許容されないと考えられて
いる。このような微量金属イオンの除去対策を講じない
場合の純水中微量金属イオン濃度とウエハ表面汚染量の
関係を調べた。その結果を表1に示す(測定方法は後述
する)。
In the high-temperature ultrapure water apparatus of Conventional Example 2, when the above-mentioned elution prevention treatment was not performed, it was confirmed that the obtained high-temperature ultrapure water contained metal ions of about 50 ppt Fe and 10 ppt Ni. I have. In a semiconductor manufacturing process, metal ions are deposited on a wafer surface at 1 × 10 10 at.
It is believed that ms / cm 2 or more is not acceptable. The relationship between the concentration of trace metal ions in pure water and the amount of contamination on the wafer surface without taking such measures to remove trace metal ions was examined. The results are shown in Table 1 (the measuring method will be described later).

【0017】[0017]

【表1】 表1より、微量金属イオン未除去の場合、純水中に49
〜67pptのFeイオンが含まれ、このFeイオン含
有純水を半導体製造工程のウエハ洗浄に使用すると、ウ
エハ表面に1.57〜8.64×1010atoms/c
2 のFeイオンが付着して該表面を汚染し、また、高
温ほどその汚染量が多くなるという問題があることがわ
かる。
[Table 1] As shown in Table 1, when trace metal ions were not removed, 49
When pure water containing Fe ions is used for cleaning a wafer in a semiconductor manufacturing process, 1.57 to 8.64 × 10 10 atoms / c
It can be seen that there is a problem that m 2 Fe ions adhere and contaminate the surface, and the higher the temperature, the greater the amount of contamination.

【0018】高温の低溶存酸素濃度の超純水には、薬液
を洗い流すだけでなく、Si表面の自然酸化膜抑制やエ
ッチング、自然酸化膜表面では金属不純物の除去効果が
あるなど、デバイスプロセス上有効であることがわかっ
ていた。しかし、従来例2の高温超純水製造装置におい
て、金属イオン溶出防止処理を実施していない場合、製
造される高温超純水中にウエハ表面を汚染して問題とな
るほどの微量金属イオンが含まれることから、最先端の
実デバイス製造のプロセスに適用するには問題があっ
た。
High-temperature ultrapure water with low dissolved oxygen concentration not only flushes out the chemical solution, but also has the effect of suppressing or etching natural oxide films on the Si surface and removing metal impurities on the natural oxide film surface. I knew it was effective. However, in the high-temperature ultrapure water manufacturing apparatus of the conventional example 2, when the metal ion elution prevention treatment is not performed, the produced high-temperature ultrapure water contains a trace amount of metal ions that can cause problems by contaminating the wafer surface. Therefore, there is a problem in applying it to the most advanced actual device manufacturing process.

【0019】半導体製造工程でのウエハ洗浄では、薬液
をバッチ方式で交換しているため次のような問題があっ
た。
In the wafer cleaning in the semiconductor manufacturing process, the following problems arise because the chemical solution is exchanged in a batch system.

【0020】・旧薬液抜き取り時間と新薬液供給時間と
温度調節時間の薬液交換時間と、薬液交換前には洗浄装
置内の工程にウエハが残らないようにしておく必要があ
り、このウエハを洗浄装置から送り出す時間が必要であ
り、この合計時間の間洗浄が停止することになり、生産
効率を低下させている。
The chemical liquid exchange time of the old chemical liquid withdrawal time, the new chemical liquid supply time, and the temperature adjustment time, and it is necessary to prevent the wafer from remaining in the process in the cleaning device before the chemical liquid exchange. It takes time to send out from the apparatus, and the washing is stopped during this total time, thereby reducing production efficiency.

【0021】・入れ替えた直後のウエハの洗浄性は良い
が、入れ替え直前のウエハの洗浄性は入れ替え直後の洗
浄性に比べ劣っており、製品仕上がりおよび製品性能に
バラツキが生じる。
Although the cleaning property of the wafer immediately after the replacement is good, the cleaning property of the wafer immediately before the replacement is inferior to the cleaning property immediately after the replacement, and the finished product and the product performance vary.

【0022】本発明の目的は、従来例1の装置に比べ
て、シリカ、有機物および溶存酸素が極めて少なく、バ
クテリアの殺菌が不要で、装置の構成が単純で、運転監
視、維持管理が楽であり、しかも、従来例2の装置では
必要な電解複合研磨および高温炉処理のような金属イオ
ン溶出防止処理を不要とすることにより、装置の製造工
程を簡略化し、装置製造コストを低減することができる
高温超純水製造装置および方法を提供することにある。
The object of the present invention is to reduce the amount of silica, organic substances and dissolved oxygen, eliminate the need for sterilization of bacteria, to simplify the construction of the apparatus, to facilitate operation monitoring, maintenance and management, as compared with the apparatus of the prior art 1. In addition, the apparatus of the prior art 2 eliminates the need for metal ion elution prevention processing such as electrolytic combined polishing and high-temperature furnace processing, which simplifies the manufacturing process of the apparatus and reduces the manufacturing cost of the apparatus. It is an object of the present invention to provide an apparatus and method for producing high-temperature ultrapure water.

【0023】本発明の他の目的は、半導体製造工程での
ウエハ洗浄において、薬液の状態を一定にし、薬液の状
態変化による製品のバラツキを少なくする薬液調製装置
および方法を提供することにある。また、本発明の他の
目的は、高温の低溶存酸素濃度の超純水をプロセス液と
して使用できるようにする薬液調製装置および方法を提
供することにある。
Another object of the present invention is to provide an apparatus and method for preparing a chemical solution, in which a state of a chemical solution is kept constant in wafer cleaning in a semiconductor manufacturing process, and variations in products due to changes in the state of the chemical solution are reduced. Another object of the present invention is to provide an apparatus and a method for preparing a chemical solution, which can use ultrapure water having a high dissolved oxygen concentration at a high temperature as a process liquid.

【0024】[0024]

【課題を解決するための手段】本発明の高温超純水製造
装置は、原水を凝集ろ過し脱気処理した前処理水、ある
いは、一次純水系で得られた一次純水を処理して高温の
超純水を得る蒸発器と、蒸発器で得られた超純水に含ま
れる微量金属イオンを除去するイオン交換装置とを備え
ているものである。
The apparatus for producing high-temperature ultrapure water according to the present invention is characterized in that raw water is subjected to coagulation filtration and deaeration treatment of pretreated water, or primary pure water obtained in a primary pure water system, and is treated with high-temperature water. And an ion exchanger for removing trace metal ions contained in the ultrapure water obtained by the evaporator.

【0025】本発明装置の一次純水系は、上記の従来例
1における一次純水系と同じものであってよく、濾過装
置、逆浸透装置、脱気装置およびイオン交換装置により
構成されている。また、本発明装置において、原水水質
によっては、一次純水系に代えて、凝集ろ過装置および
脱気装置より構成された前処理系を用いてもよい。
The primary pure water system of the device of the present invention may be the same as the primary pure water system in the above-mentioned conventional example 1, and is constituted by a filtration device, a reverse osmosis device, a deaerator and an ion exchange device. In the apparatus of the present invention, depending on the quality of raw water, a pretreatment system including a coagulation filtration device and a deaeration device may be used instead of the primary pure water system.

【0026】蒸発器は、上記の従来例2におけるものと
同じであってよく、上記前処理系で得られた前処理水、
あるいは、一次純水系で得られた一次純水を処理して高
温超純水を得る多重効用蒸発器(I) を主体とし、その後
流に必要に応じて限外濾過(UF)装置(2) を備えたも
のである。蒸発器は100℃程度の高温で操作される。
ただし、蒸発器を構成する金属材料には、金属イオン溶
出防止処理が施されていなくてよい。
The evaporator may be the same as that in the conventional example 2 described above, and the pretreated water obtained in the pretreatment system,
Alternatively, a multi-effect evaporator (I) for treating primary pure water obtained in a primary pure water system to obtain high-temperature ultrapure water is mainly used, and an ultrafiltration (UF) device (2) is provided in the subsequent stream as necessary. It is provided with. The evaporator is operated at a high temperature of the order of 100 ° C.
However, the metal material constituting the evaporator may not be subjected to the metal ion elution prevention treatment.

【0027】イオン交換装置が、混床式イオン交換樹脂
または強酸性陽イオン交換樹脂(カチオン交換樹脂)を
充填していることが好ましい。これらの混床式イオン交
換樹脂および強酸性陽イオン交換樹脂としては、耐熱性
を有するものが好ましい。混床式イオン交換樹脂は、強
酸性陽イオン交換樹脂と強塩基性陰イオン交換樹脂を所
要の交換容量比で混合充填したものである。蒸発器で得
られた高温超純水は、高温のまま、または、生産水熱交
換器と冷却熱交換器で40℃以下まで冷却して、これら
のイオン交換樹脂に供給される。混床式イオン交換樹脂
としては、強酸性陽イオン交換樹脂と強塩基性陰イオン
交換樹脂を交換容量比1:1で混合充填したもの、例え
ば三菱化学製のイオン交換樹脂SMT100が例示さ
れ、また強酸性陽イオン交換樹脂としては、三菱化学製
のイオン交換樹脂SKT10が例示される。
It is preferable that the ion exchange apparatus is filled with a mixed bed type ion exchange resin or a strongly acidic cation exchange resin (cation exchange resin). As these mixed bed type ion exchange resins and strongly acidic cation exchange resins, those having heat resistance are preferable. The mixed bed type ion exchange resin is obtained by mixing and filling a strongly acidic cation exchange resin and a strongly basic anion exchange resin at a required exchange capacity ratio. The high-temperature ultrapure water obtained in the evaporator is supplied to these ion-exchange resins as they are at a high temperature or cooled to 40 ° C. or less by a production water heat exchanger and a cooling heat exchanger. Examples of the mixed-bed ion exchange resin include a mixture obtained by mixing and filling a strongly acidic cation exchange resin and a strongly basic anion exchange resin at an exchange capacity ratio of 1: 1 such as an ion exchange resin SMT100 manufactured by Mitsubishi Chemical Corporation. An example of the strong acidic cation exchange resin is an ion exchange resin SKT10 manufactured by Mitsubishi Chemical.

【0028】イオン交換装置としては、イオン交換樹脂
の替わりにイオン交換膜またはイオン交換繊維あるいは
イオン交換膜とイオン交換繊維を充填したものでも良
い。イオン交換膜とイオン交換繊維としては、耐熱性を
有するものが好ましい。
The ion exchange apparatus may be an ion exchange membrane, an ion exchange fiber, or an ion exchange membrane and an ion exchange fiber filled with ion exchange fibers instead of the ion exchange resin. As the ion exchange membrane and the ion exchange fiber, those having heat resistance are preferable.

【0029】さらに、イオン交換装置として、連続通水
型電気脱イオン装置を備えたものでも良い。連続通水型
電気脱イオン装置の例を図6から図8までに示す。図6
に示す連続通水型電気脱イオン装置(50)は、陽イオン交
換膜(53)および陰イオン交換膜(54)で形成された被処理
水水路(52)に、陽イオン交換樹脂(55)と陰イオン交換樹
脂(56)が充填されていて、さらに陽イオン交換膜(53)の
外側に陰イオン交換膜(57)を、陰イオン交換膜(54)の外
側に陽イオン交換膜(58)を備えた濃縮水水路(59)が形成
されおり、濃縮水水路(59)の外側に電界を印加すること
により連続イオン交換処理を可能としたものであり、栗
田工業(株)製CDIが例示される。図7に示す連続通
水型電気脱イオン装置(51)は、図6に示す連続通水型電
気脱イオン装置(50)において、すべての水路(52)(59)に
イオン交換樹脂(55)(56)を充填するとともに、中央の水
路を濃縮水水路(59)、これの外側の水路を被処理水水路
(52)としたものであり、栗田工業(株)製新型CDIが
例示される。また、図8に示す連続通水型電気脱イオン
装置(61)は、陽イオン交換膜(63)および陰イオン交換膜
(64)で形成された被処理水水路(62)に、陽イオン交換繊
維(65)と陰イオン交換繊維(66)が充填されているもの
で、日本錬水(株)製New Codesが例示され
る。連続通水型電気脱イオン装置のイオン交換体として
は、それぞれ耐熱性を有するイオン交換樹脂およびイオ
ン交換繊維が好ましい。
Further, as the ion exchange device, a device provided with a continuous water passing type electrodeionization device may be used. FIGS. 6 to 8 show examples of the continuous water flow type electrodeionization apparatus. FIG.
The continuous water passing type electrodeionization device (50) shown in (5) is a cation exchange resin (55) in the water channel to be treated (52) formed by the cation exchange membrane (53) and the anion exchange membrane (54). And an anion exchange resin (56), an anion exchange membrane (57) outside the cation exchange membrane (53), and a cation exchange membrane (58) outside the anion exchange membrane (54). A concentrated water channel (59) provided with a concentrated water channel (59) is formed, and continuous ion exchange treatment is enabled by applying an electric field to the outside of the concentrated water channel (59). Is exemplified. The continuous water passing type electrodeionization device (51) shown in FIG. 7 is different from the continuous water passing type electrodeionization device (50) shown in FIG. 6 in that all the water channels (52) and (59) have ion exchange resins (55). (56), the central channel is a concentrated water channel (59), and the outer channel is a treated channel.
(52), for example, a new CDI manufactured by Kurita Water Industries Ltd. Further, the continuous water passing type electrodeionization device (61) shown in FIG. 8 includes a cation exchange membrane (63) and an anion exchange membrane.
The water channel (62) to be treated formed in (64) is filled with cation exchange fibers (65) and anion exchange fibers (66), for example, New Codes manufactured by Nippon Rensui Co., Ltd. Is done. As the ion exchanger of the continuous water passing type electrodeionization apparatus, an ion exchange resin and an ion exchange fiber each having heat resistance are preferable.

【0030】本発明の高温超純水製造装置によると、先
ず、前処理系あるいは一次純水系により原水(工業用水
または市水)が処理され、原水中の懸濁物質、電解物
質、微粒子、微生物等が除去される。しかし、前処理系
あるいは一次純水系の処理だけでは、シリカや有機物な
どの非イオン性不純物の除去性能および溶存酸素の除去
が不十分であり、これらの除去を目的として、前処理水
あるいは一次純水が蒸発器に供給されて処理される。蒸
発器での純水製造プロセスは、相変化と抽気操作を伴う
ため、シリカや有機物などの非イオン性不純物、溶存酸
素などの溶存気体も極微量となるまで分離除去される。
蒸発器には、接液部の電解複合研磨や高温炉での強制酸
化皮膜処理といった金属イオン溶出防止処理が施されて
いないので、蒸発器で得られた高温超純水には、微量の
金属イオンが含まれることになるが、この微量金属イオ
ンは、イオン交換装置の混床式イオン交換樹脂または強
酸性陽イオン交換樹脂により除去される。こうして得ら
れた高温の超純水は、例えばウエハ洗浄用に用いられ
る。
According to the apparatus for producing high-temperature ultrapure water of the present invention, first, raw water (industrial water or city water) is treated by a pretreatment system or a primary pure water system, and suspended substances, electrolytic substances, fine particles, microorganisms and the like in the raw water are treated. Etc. are removed. However, the treatment of the pretreatment system or the primary pure water system alone is insufficient in the performance of removing nonionic impurities such as silica and organic substances and the removal of dissolved oxygen. Water is supplied to the evaporator for treatment. Since the process of producing pure water in the evaporator involves a phase change and a bleeding operation, non-ionic impurities such as silica and organic substances, and dissolved gases such as dissolved oxygen are also separated and removed until they become extremely small.
The evaporator is not subjected to metal ion elution prevention treatment such as electrolytic combined polishing of the liquid contact part and forced oxide film treatment in a high-temperature furnace. Although the ions are included, the trace metal ions are removed by the mixed bed type ion exchange resin or the strongly acidic cation exchange resin of the ion exchange device. The high-temperature ultrapure water thus obtained is used, for example, for cleaning a wafer.

【0031】本発明の高温超純水製造装置は、蒸発器で
得られた高温の微量金属イオン未除去超純水とイオン交
換装置で処理された常温の微量金属イオン除去済み超純
水とを熱交換することにより、上記高温の微量金属イオ
ン未除去超純水をイオン交換装置への供給前に冷却する
とともに、常温の微量金属イオン除去済み超純水を加熱
する生産水熱交換器をさらに備えていることが好まし
い。
The apparatus for producing high-temperature ultrapure water of the present invention is characterized in that ultrapure water of high temperature with no trace metal ions removed by the evaporator and ultrapure water of normal temperature with trace metal ions removed by the ion exchanger are removed. By performing heat exchange, the high-temperature trace metal ion non-removed ultrapure water is cooled before being supplied to the ion exchanger, and a production water heat exchanger for heating the room temperature trace metal ion-removed ultrapure water is further provided. Preferably, it is provided.

【0032】また、本発明の高温超純水製造装置は、生
産水熱交換器で冷却された微量金属イオン未除去超純水
を40℃以下まで冷却してイオン交換装置への供給水と
する冷却熱交換器をさらに備えていることが好ましい。
Further, the high-temperature ultrapure water producing apparatus of the present invention cools ultrapure water from which trace metal ions have not been removed cooled by the production water heat exchanger to 40 ° C. or less to supply water to the ion exchange apparatus. It is preferable to further include a cooling heat exchanger.

【0033】上記の熱交換器は、蒸発器、生産水熱交換
器、冷却熱交換器およびイオン交換装置が、上流側から
この順となるように配置される。上記熱交換器は、従来
の超純水の熱交換器に使用されているPFAやPVDF
等の溶出の少ないふっ素樹脂で製作されているものであ
ってもよい。
In the above heat exchanger, the evaporator, the production water heat exchanger, the cooling heat exchanger, and the ion exchanger are arranged in this order from the upstream side. The heat exchanger is a PFA or PVDF used in a conventional heat exchanger of ultrapure water.
It may be made of a fluororesin with little elution such as.

【0034】生産水熱交換器に金属材料を使用する場
合、生産水熱交換器は金属材料の純水中への溶出に対し
て厳しい条件の高温度領域で使用され、微量金属イオン
除去済みの常温超純水を加熱するものであるので、金属
の中で最も溶出の少ないチタン製、電解研磨後特殊熱処
理をした酸化不動態ステンレス鋼製または電解複合研磨
後特殊熱処理をした酸化不動態ステンレス鋼製のものが
好ましい。電解研磨後特殊熱処理をした酸化不動態ステ
ンレス鋼としては、神鋼パンテック(株)製GOLD
EP WHITE が例示される。
When a metal material is used in the production water heat exchanger, the production water heat exchanger is used in a high temperature region under severe conditions for elution of the metal material into pure water, and a trace metal ion is removed. Heats room-temperature ultrapure water, so it is made of titanium, which is the least eluted metal, and is made of oxidation-passive stainless steel that has been subjected to special heat treatment after electrolytic polishing or has been subjected to special heat treatment after electrolytic combined polishing. Is preferred. GOLD manufactured by Shinko Pantech Co., Ltd. is an oxidation passivated stainless steel that has been subjected to special heat treatment after electrolytic polishing.
EP WHITE is exemplified.

【0035】冷却熱交換器に金属材料を使用する場合、
冷却熱交換器は金属材料の純水中への溶出に対してそれ
ほど厳しくない条件の中温度領域で使用され、イオン交
換装置に通水される前の超純水を冷却するものであるの
で、ステンレス鋼と同等かより純水への溶出量が少ない
金属材料のものが好ましい。冷却熱交換器の金属材料と
しては、例えばステンレス鋼、チタン、電解研磨後特殊
熱処理をした酸化不動態ステンレス鋼または電解複合研
磨後特殊熱処理をした酸化不動態ステンレス鋼などが例
示される。
When using a metal material for the cooling heat exchanger,
Since the cooling heat exchanger is used in a medium temperature range under conditions where the elution of metallic materials into pure water is not so severe, it cools ultrapure water before being passed through the ion exchange device. It is preferable to use a metal material having the same or lower elution amount to pure water than stainless steel. Examples of the metal material of the cooling heat exchanger include, for example, stainless steel, titanium, oxidation passivated stainless steel subjected to special heat treatment after electrolytic polishing, and oxide passivated stainless steel subjected to special heat treatment after electrolytic composite polishing.

【0036】上記の高温超純水製造装置により得られる
高温超純水は、図5に示す半導体製造プロセスの処理工
程において、超純水リンス時にそのまま使用されるのは
もちろんのことであるが、本発明の薬液調製装置によっ
て、高温超純水を電解イオン水としたり、高温超純水に
NH4 OH、H2 2 、HCl、HF、H2 SO4 、H
NO3 などの薬剤(「薬剤」という語は、薬液原液だけ
でなく、材料ガスおよび酸化系ガスなども含むものとす
る)を混合することにより、半導体製造プロセスの処理
工程のリンス以外で使用される薬液を得ることもでき
る。
The high-temperature ultrapure water obtained by the above-mentioned high-temperature ultrapure water production apparatus is used as it is at the time of rinsing the ultrapure water in the processing steps of the semiconductor production process shown in FIG. the drug solution preparing apparatus of the present invention, or a high-temperature ultra-pure water and the electrolytic ion water, NH 4 OH to a high temperature ultra-pure water, H 2 O 2, HCl, HF, H 2 SO 4, H
By mixing a chemical such as NO 3 (the term “chemical” includes not only a raw chemical solution but also a material gas and an oxidizing gas), a chemical solution used in a process other than rinsing in a processing step of a semiconductor manufacturing process. You can also get

【0037】本発明(請求項10)の薬液調製装置は、
本発明の高温超純水製造装置と、高温超純水製造装置に
より得られた高温超純水を電解アノード水と電解カソー
ド水とに分解する電界イオン水製造装置と、電解アノー
ド水および電解カソード水を直接半導体もしくはその他
の精密デバイスの処理装置の薬液槽に供給する供給装置
とを備えているものである。高温超純水を高温のまま電
解イオン水製造装置に通水することにより、高温の電解
イオン水(電解アノード水と電解カソード水)が得られ
る。電解アノード水および電解カソード水は、異なる薬
液槽に供給される。電解イオン水製造装置としては、オ
ルガノ(株)製の三槽式電解槽の構造を持つ電解イオン
水製造装置が例示される。三槽式電解槽に用いられるイ
オン交換膜やイオン交換樹脂は、耐熱性を有するものが
好ましい。
The chemical solution preparation device of the present invention (claim 10)
High-temperature ultrapure water production apparatus of the present invention, an electric field ion water production apparatus for decomposing high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus into electrolytic anode water and electrolytic cathode water, electrolytic anode water and electrolytic cathode A supply device for directly supplying water to a chemical solution tank of a processing device of a semiconductor or other precision device. By passing the high-temperature ultrapure water through the electrolytic ionic water producing apparatus at a high temperature, high-temperature electrolytic ionic water (electrolytic anode water and electrolytic cathode water) can be obtained. Electrolytic anode water and electrolytic cathode water are supplied to different chemical tanks. As the electrolytic ionic water producing apparatus, an electrolytic ionic water producing apparatus having a three-tank type electrolytic cell structure manufactured by Organo Corporation is exemplified. The ion exchange membrane and the ion exchange resin used in the three-tank electrolytic cell preferably have heat resistance.

【0038】本発明(請求項11)の薬液調製装置は、
本発明の高温超純水製造装置と、高温超純水製造装置に
より得られた高温超純水および高温超純水に混合される
薬剤を半導体もしくはその他の精密デバイスの処理装置
の薬液槽に直接供給するとともに、薬液槽内の薬液が所
望の温度あるいは濃度となるように調整する薬液供給調
整装置とを備えているものである(図12参照)。薬液
槽内の薬液が所望の濃度となるようにする構成として、
例えば、高温超純水定量供給装置および自動薬液原液供
給装置が設けられる。高温超純水定量供給装置は、指示
調節計、出力付きの流量計、自動調節弁を備えている。
また、自動薬液原液供給装置は、薬液原液タンク、指示
調節計、出力付きの流量計、自動調節弁等を備えてい
る。薬液槽内の薬液が所望の温度となるようにする構成
として、例えば熱交換器がさらに設けられる。
According to the present invention (claim 11),
The high-temperature ultrapure water production apparatus of the present invention, and the high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus and the agent mixed with the high-temperature ultrapure water are directly supplied to a chemical solution tank of a semiconductor or other precision device processing apparatus. It is provided with a chemical liquid supply adjusting device for adjusting the supply of the chemical liquid in the chemical liquid tank to a desired temperature or concentration (see FIG. 12). As a configuration to make the chemical solution in the chemical tank have a desired concentration,
For example, a high-temperature ultrapure water fixed-quantity supply device and an automatic stock solution supply device are provided. The high-temperature ultrapure water quantitative supply device includes an indicating controller, a flow meter with an output, and an automatic control valve.
Further, the automatic chemical liquid feeder is provided with a chemical liquid tank, an indicator controller, a flow meter with output, an automatic control valve, and the like. For example, a heat exchanger is further provided as a configuration for adjusting the temperature of the chemical in the chemical bath to a desired temperature.

【0039】本発明(請求項12)の薬液調製装置は、
本発明の高温超純水製造装置と、高温超純水製造装置に
より得られた高温超純水に薬剤を混合する混合装置とを
備えているものである。混合装置としては、例えばミキ
サーが用いられ、ミキサー内の薬液が所望の濃度となる
ようにする構成として、例えば、上記の高温超純水定量
供給装置および自動薬液原液供給装置が設けられる(図
10および図11参照)。薬液槽内の薬液が所望の温度
となるようにする構成として、例えば熱交換器が薬液槽
とミキサーとの間に設けられる(図10参照)。ミキサ
ーは、高温超純水製造装置近傍に設けても良いし、薬液
槽の近傍に設けても良い。また、自動薬液原液供給装置
に替えてガス供給装置(図示略)を設け、高温超純水製
造装置により得られた高温超純水に、HCl、NH3
HF、NH4 F、SOx、NOx等の材料ガスやO3
2 、酸素ラジカルなどの酸化系ガスを混合することに
より、薬液を得るようにしてもよい。
The chemical solution preparation device of the present invention (claim 12) is
The apparatus comprises a high-temperature ultrapure water production apparatus according to the present invention and a mixing apparatus for mixing a drug into the high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus. As the mixing device, for example, a mixer is used, and as a configuration for making the chemical solution in the mixer have a desired concentration, for example, the above-described high-temperature ultrapure water constant-quantity supply device and the automatic chemical solution supply device are provided (FIG. 10). And FIG. 11). For example, a heat exchanger is provided between the chemical solution tank and the mixer as a configuration for adjusting the temperature of the chemical solution in the chemical solution tank to a desired temperature (see FIG. 10). The mixer may be provided near the high-temperature ultrapure water production apparatus, or may be provided near the chemical solution tank. In addition, a gas supply device (not shown) is provided in place of the automatic chemical stock solution supply device, and HCl, NH 3 , and the like are added to the high-temperature ultrapure water obtained by the high-temperature ultrapure water production device.
Material gases such as HF, NH 4 F, SOx, NOx, O 3 ,
A chemical solution may be obtained by mixing an oxidizing gas such as O 2 and oxygen radicals.

【0040】また、薬液調製装置により得られた薬液を
薬液槽に供給する方法には、所望の濃度でかつ所望の温
度とした薬液を薬液槽にバッチ方式で供給する方法と、
所望の濃度でかつ所望の温度とした薬液を所定量で連続
して薬液槽に供給するとともに、供給量と同等の量を薬
液槽から抜き出す方法とがある。
The method of supplying the chemical solution obtained by the chemical solution preparation device to the chemical solution tank includes a method of supplying a chemical solution having a desired concentration and a desired temperature to the chemical solution tank in a batch method.
There is a method in which a chemical solution having a desired concentration and a desired temperature is continuously supplied in a predetermined amount to a chemical solution tank, and an amount equivalent to the supply amount is extracted from the chemical solution tank.

【0041】[0041]

【発明の実施例】以下に本発明の高温超純水製造装置の
具体例を図1および図2に基づいて説明する。ただし、
本発明はこれらのものに限定されるものではない。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the high-temperature ultrapure water production apparatus according to the present invention will be described below with reference to FIGS. However,
The present invention is not limited to these.

【0042】図1は、本発明の高温超純水製造装置の第
1実施例を示している。同図に示すように、この高温超
純水製造装置は、工業用水または市水(上水道水)を原
水として処理し一次純水を得る一次純水系(21)と、一次
純水系(21)で得られた一次純水を処理して高温超純水を
得る多重効用蒸発器(22)と、蒸発器(22)で得られた高温
超純水に含まれる微量金属イオンを除去するイオン交換
装置(23)と、蒸発器(22)とイオン交換装置(23)との間に
設けられた生産水熱交換器(24)および冷却熱交換器(25)
とよりなる。
FIG. 1 shows a first embodiment of a high-temperature ultrapure water producing apparatus according to the present invention. As shown in the figure, this high-temperature ultrapure water production system is composed of a primary pure water system (21), which obtains primary pure water by treating industrial water or city water (tap water) as raw water, and a primary pure water system (21). A multiple-effect evaporator (22) that processes the obtained primary pure water to obtain high-temperature ultrapure water, and an ion exchange device that removes trace metal ions contained in the high-temperature ultrapure water obtained by the evaporator (22) (23), a production water heat exchanger (24) and a cooling heat exchanger (25) provided between the evaporator (22) and the ion exchanger (23).
And

【0043】一次純水系(21)は、濾過装置、逆浸透装
置、脱気装置およびイオン交換装置により構成されてお
り(図3参照)、常温(例えば25℃)で供給された工
業用水または市水(上水道水)を原水として処理し、常
温の一次純水を得、これを蒸発器(22)に供給する。一次
純水系(21)では、懸濁物質は濾過装置で、電解(イオ
ン)物質は逆浸透装置とイオン交換装置で、溶存酸素は
脱気装置で主に除去され、抵抗率17.5MΩ・cm、
微量金属イオン0.1ppb(100ppt)、TOC
30ppb、シリカ(SiO2 )3ppb、溶存酸素5
0ppb程度の純水が得られる。
The primary pure water system (21) is composed of a filtration device, a reverse osmosis device, a deaerator and an ion exchange device (see FIG. 3), and is supplied with industrial water or city water supplied at normal temperature (for example, 25 ° C.). Water (tap water) is treated as raw water to obtain room temperature primary pure water, which is supplied to an evaporator (22). In the primary pure water system (21), the suspended substance is mainly removed by a filtration device, the electrolytic (ion) material is removed by a reverse osmosis device and an ion exchange device, and the dissolved oxygen is mainly removed by a deaeration device, and the resistivity is 17.5 MΩ · cm. ,
Trace metal ion 0.1ppb (100ppt), TOC
30 ppb, silica (SiO 2 ) 3 ppb, dissolved oxygen 5
Pure water of about 0 ppb is obtained.

【0044】イオン交換装置(23)には、強酸性陽イオン
交換樹脂(三菱化学製のイオン交換樹脂SKT10)が
充填されている。
The ion exchange unit (23) is filled with a strongly acidic cation exchange resin (ion exchange resin SKT10 manufactured by Mitsubishi Chemical Corporation).

【0045】蒸発器(22)は、図4に示した従来例2のも
のと同じ構成のものであり、一次純水系で得られた一次
純水を処理して高温超純水を得る多重効用蒸発器を主体
とする。ただし、蒸発器を構成する金属材料には、金属
イオン溶出防止処理が施されていない。一次純水をこの
蒸発器(22)に供給することにより、従来例2と同じプロ
セスによって約75℃の高温超純水が得られる。得られ
た高温超純水は、表2に示すように、蒸発器構成金属材
料の金属イオン(FeイオンおよびNiイオン)を微量
含む以外は非常に純度の高い高温超純水である。
The evaporator (22) has the same structure as that of the conventional example 2 shown in FIG. 4, and has a multiple effect of treating primary pure water obtained in a primary pure water system to obtain high-temperature ultrapure water. Mainly evaporator. However, the metal material constituting the evaporator has not been subjected to the metal ion elution prevention treatment. By supplying the primary pure water to the evaporator (22), high-temperature ultrapure water of about 75 ° C. is obtained by the same process as in the conventional example 2. As shown in Table 2, the obtained high-temperature ultrapure water is extremely high-purity ultrapure water except that it contains a small amount of metal ions (Fe ions and Ni ions) of the metal material constituting the evaporator.

【0046】[0046]

【表2】 蒸発器(22)で得られた高温超純水は、生産水熱交換器(2
4)の高温流体側入口に送られてここで40℃程度まで冷
却され、次いで、冷却熱交換器(25)の高温流体側入口に
送られてここで35℃程度までさらに冷却されてから、
イオン交換装置(23)に通される。そして、イオン交換装
置(23)により、蒸発器(22)で得られた高温超純水に含ま
れる微量金属イオン(FeイオンおよびNiイオン)が
除去される。イオン交換装置(23)を通過した超純水は、
温度35℃で抵抗率18.0MΩ・cm以上、微量金属
イオン5ppt以下の常温超純水となる。この常温超純
水は、生産水熱交換器(24)の低温流体側入口に送られ、
ここで、蒸発器(22)で得られた75℃の高温超純水の熱
を回収して、温度70℃で抵抗率18.0MΩ・cm以
上、微量金属イオン5ppt以下の高温超純水として低
温流体側出口より出る。この高温超純水は、ウエハ洗浄
用高温超純水としてユースポイントに送られる。
[Table 2] The high-temperature ultrapure water obtained in the evaporator (22) is supplied to the production water heat exchanger (2
4) sent to the high temperature fluid side inlet and cooled here to about 40 ° C., and then sent to the high temperature fluid side inlet of the cooling heat exchanger (25) and further cooled to about 35 ° C.
It is passed through the ion exchange device (23). Then, trace metal ions (Fe ions and Ni ions) contained in the high-temperature ultrapure water obtained in the evaporator (22) are removed by the ion exchange device (23). Ultrapure water that has passed through the ion exchange device (23)
It becomes ultrapure water at room temperature with a resistivity of 18.0 MΩ · cm or more and a trace metal ion of 5 ppt or less at a temperature of 35 ° C. This room-temperature ultrapure water is sent to the low-temperature fluid side inlet of the production water heat exchanger (24),
Here, the heat of the high-temperature ultrapure water at 75 ° C. obtained by the evaporator (22) is recovered and converted into high-temperature ultrapure water having a resistivity of 18.0 MΩ · cm or more and a trace metal ion of 5 ppt or less at a temperature of 70 ° C. Exit from the low temperature fluid side outlet. This high-temperature ultrapure water is sent to a use point as high-temperature ultrapure water for wafer cleaning.

【0047】冷却熱交換器(25)の低温流体側には、例え
ば、冷却塔からの冷却水が供給されるが、冷却水とし
て、チラー装置からの冷水を用いても良い。生産水熱交
換器(24)において30〜45℃の中温まで冷却された微
量金属イオン未除去超純水は、冷却熱交換器(25)により
さらに冷却される。イオン交換装置(23)に充填されるイ
オン交換樹脂が耐熱性を有していない場合、イオン交換
装置(23)通過前の微量金属イオン未除去超純水の温度は
好ましくは40℃以下であるが、冷却熱交換器(25)を設
置することにより、この温度が保証される。生産水熱交
換器(24)を通過後の微量金属イオン未除去超純水の温度
がイオン交換樹脂の耐熱温度以下である場合、冷却熱交
換器(25)は設置しなくてもよい。
The low-temperature fluid side of the cooling heat exchanger (25) is supplied with, for example, cooling water from a cooling tower. As the cooling water, cold water from a chiller device may be used. The ultrapure water from which trace metal ions have not been removed and which has been cooled to a medium temperature of 30 to 45 ° C. in the production water heat exchanger (24) is further cooled by the cooling heat exchanger (25). When the ion exchange resin to be filled in the ion exchange device (23) does not have heat resistance, the temperature of the ultrapure water without removing trace metal ions before passing through the ion exchange device (23) is preferably 40 ° C or less. However, by installing a cooling heat exchanger (25), this temperature is guaranteed. If the temperature of the ultrapure water from which the trace metal ions have not been removed after passing through the production water heat exchanger (24) is equal to or lower than the heat resistant temperature of the ion exchange resin, the cooling heat exchanger (25) may not be provided.

【0048】上記において、生産水熱交換器(24)はチタ
ン製、冷却熱交換器(25)はSUS316製である。
In the above, the production water heat exchanger (24) is made of titanium, and the cooling heat exchanger (25) is made of SUS316.

【0049】冷却熱交換器(25)に通される超純水は、生
産水熱交換器(24)により冷却されて、金属材料の溶出に
対してそれほど厳しくない条件の中温度領域となってお
り、冷却熱交換器(25)をSUS316製としても、微量
金属イオンが溶出することはほとんどない。また、冷却
熱交換器(25)から微量金属イオンが超純水中に極微量溶
出したとしても、超純水がこの後にイオン交換装置(23)
を通過するので、溶出金属イオンが問題となることはな
い。したがって、冷却熱交換器(25)の金属材料として
は、純水への溶出量がステンレス鋼と同等かそれ以下の
もの、例えばSUS316、SUS316L、SUS3
04、SUS304Lおよびこれらと同等の溶出特性を
有するその他のステンレス鋼、チタン、電解研磨後特殊
熱処理をした酸化不動態ステンレス鋼または電解複合研
磨後特殊熱処理をした酸化不動態ステンレス鋼などが考
えられる。
The ultrapure water passed through the cooling heat exchanger (25) is cooled by the production water heat exchanger (24) to become a medium temperature region under conditions that are not so severe for elution of metallic materials. Therefore, even if the cooling heat exchanger (25) is made of SUS316, trace metal ions hardly elute. Also, even if trace amounts of metal ions elute from the cooling heat exchanger (25) into ultrapure water, the ultrapure water is
, So that the eluting metal ions are not a problem. Therefore, as the metal material of the cooling heat exchanger (25), the elution amount to pure water is equal to or less than that of stainless steel, for example, SUS316, SUS316L, SUS3
04, SUS304L, and other stainless steels having the same elution characteristics as those of stainless steel, titanium, oxidation passivated stainless steel subjected to special heat treatment after electrolytic polishing, or oxidation passivated stainless steel subjected to special heat treatment after electrolytic composite polishing.

【0050】一方、生産水熱交換器(24)は、金属材料の
溶出に対して厳しい条件の高温度領域で使用され、ま
た、生産水熱交換器(24)に通された微量金属イオン除去
済み超純水は、そのまま、洗浄水として使用されること
になる。そこで、生産水熱交換器(24)を金属イオン溶出
がほとんど無いチタン製熱交換器とすることにより、最
終的に得られる高温の超純水の水質の悪化が防止され
る。生産水熱交換器(24)の金属材料としては、チタンの
他、電解研磨後特殊熱処理をした酸化不動態ステンレス
鋼または電解複合研磨後特殊熱処理をした酸化不動態ス
テンレス鋼などが考えられる。
On the other hand, the production water heat exchanger (24) is used in a high temperature region under severe conditions for elution of metallic materials, and removes trace metal ions passed through the production water heat exchanger (24). The used ultrapure water is used as it is as washing water. Therefore, by making the production water heat exchanger (24) a titanium heat exchanger with almost no metal ion elution, deterioration of the quality of the finally obtained high-temperature ultrapure water is prevented. As the metal material of the production water heat exchanger (24), in addition to titanium, oxidized passivated stainless steel subjected to special heat treatment after electrolytic polishing or oxidized passivated stainless steel subjected to special heat treatment after electrolytic combined polishing, and the like can be considered.

【0051】本発明の高温超純水製造装置のイオン交換
装置(23)出口(35℃)と、その後流のチタン製生産水
熱交換器(24)出口(70℃)における水質を分析した。
その結果を表3に示す。
The water quality at the outlet (35 ° C.) of the ion exchanger (23) and the outlet (70 ° C.) of the titanium-made production water heat exchanger (24) downstream of the high-temperature ultrapure water production apparatus of the present invention was analyzed.
Table 3 shows the results.

【0052】[0052]

【表3】 本発明の高温超純水製造装置で得られた超純水を用い
て、純水浸漬テストおよび半導体製造工程で実施されて
いるウエット洗浄工程を模擬したコンタミネーション確
認テストを行い、ウエハの表面分析を行った。その結果
を表4に示す。
[Table 3] Using ultrapure water obtained by the high temperature ultrapure water production apparatus of the present invention, a pure water immersion test and a contamination confirmation test simulating a wet cleaning process performed in a semiconductor production process are performed, and a wafer surface analysis is performed. Was done. Table 4 shows the results.

【0053】[0053]

【表4】 表4より、常温よりも金属イオン汚染に対して厳しい高
温の場合でも、Feイオンは半導体製造工程で許容でき
ないと考えられている1×1010atoms/cm2
下であり、問題とならないレベルとなっており、従って
本発明の高温超純水製造装置で製造した高温超純水が、
半導体製造工程のウエハ洗浄に適していることがわか
る。また、冷却熱交換器(25)にSUS製熱交換器を、生
産水熱交換器(24)にチタン熱交換器を用いても問題ない
こともわかる。
[Table 4] From Table 4, it can be seen that even at a high temperature, which is more severe against metal ion contamination than at room temperature, Fe ions are 1 × 10 10 atoms / cm 2 or less, which is considered to be unacceptable in the semiconductor manufacturing process. Has become, therefore, high-temperature ultrapure water produced by the high-temperature ultrapure water production apparatus of the present invention,
It can be seen that it is suitable for wafer cleaning in a semiconductor manufacturing process. It can also be seen that there is no problem if a SUS heat exchanger is used for the cooling heat exchanger (25) and a titanium heat exchanger is used for the production water heat exchanger (24).

【0054】なお、表4および前述の表1において、純
水中のFe濃度測定は、セイコー電子工業製SPQ−8
000(高感度仕様)を用いた誘導結合プラズマ質量分
析法により、また、ウエハ表面のFe分析は、(株)テ
クノス製TREX610Tを用いた全反射蛍光X線分析
法によりそれぞれ行ったものである。
In Table 4 and Table 1 described above, the Fe concentration in pure water was measured using SPQ-8 manufactured by Seiko Denshi Kogyo.
000 (high sensitivity specification) was performed by inductively coupled plasma mass spectrometry, and the Fe analysis of the wafer surface was performed by total reflection X-ray fluorescence analysis using TREX610T manufactured by Technos Co., Ltd.

【0055】純水浸漬テストの測定には、テストピース
として、所定温度(常温および高温)の純水のオーバー
フロー水槽中に浸漬した後、スピンドライヤーで乾燥さ
せたウエハを用い、RCAテストの常温リンス条件での
測定には、テストピースとして、ウエハをH2 SO4
2 2 溶液に浸漬、常温純水のオーバーフロー水槽中
に浸漬、NH4 OH/H2 2 /H2 O溶液に浸漬、常
温純水のオーバーフロー水槽中に浸漬、HCl/H2
2 /H2 O溶液に浸漬した後、さらに、常温純水のオー
バーフロー水槽中に浸漬した後、スピンドライヤーで乾
燥させたものを用いた。RCAテストの高温リンス条件
での測定には、RCAテストの常温純水を高温純水に代
えた以外は上記常温リンス条件での測定と同じ操作を繰
り返した。RCA+HFテストの常温リンス条件での測
定には、テストピースとして、RCAの上記常温リンス
条件と同じ条件で処理したウエハをさらに希フッ酸溶液
に浸漬し、常温純水のオーバーフロー水槽中に浸漬した
後、スピンドライヤーで乾燥させたものを用い、また、
RCA+HFテストの高温リンス条件での測定には、テ
ストピースとして、RCAの上記高温リンス条件と同じ
条件で処理したウエハをさらに希フッ酸溶液に浸漬し、
高温純水のオーバーフロー水槽中に浸漬した後、スピン
ドライヤーで乾燥させたものを用いた。
For the measurement of the pure water immersion test, a wafer which was immersed in a pure water overflow water tank at a predetermined temperature (normal temperature and high temperature) and dried by a spin dryer was used as a test piece, and a normal temperature rinse of the RCA test was performed. For the measurement under the conditions, the wafer was used as a test piece and H 2 SO 4 /
Immersed in the H 2 O 2 solution, immersed in the overflow water bath at room temperature pure water, NH4 OH / H 2 O 2 / H 2 O solution dipping, dipped into the overflow tank cold deionized water, HCl / H 2 O
After being immersed in a 2 / H 2 O solution, further immersed in an overflow bath of room temperature pure water, and dried with a spin drier. For the measurement under the high-temperature rinsing condition of the RCA test, the same operation as the measurement under the normal-temperature rinsing condition was repeated, except that the high-temperature pure water was used instead of the normal-temperature pure water in the RCA test. For measurement under the normal temperature rinsing condition of the RCA + HF test, a wafer treated as the test piece under the same conditions as the normal temperature rinsing condition of RCA is further immersed in a dilute hydrofluoric acid solution, and then immersed in an overflow water bath of normal temperature pure water. , Using a dried with a spin dryer,
In the measurement under the high-temperature rinsing condition of the RCA + HF test, a wafer treated under the same conditions as the high-temperature rinsing condition of the RCA is further immersed in a dilute hydrofluoric acid solution as a test piece.
After being immersed in an overflow water bath of high-temperature pure water, a product dried by a spin dryer was used.

【0056】図2は、本発明の高温超純水製造装置の第
2実施例を示している。この高温超純水製造装置が第1
実施例と異なる点は、2つの熱交換器(24)(25)がともに
省略されている点にあり、これに伴って、イオン交換装
置(26)に充填される混床式イオン交換樹脂または強酸性
陽イオン交換樹脂は、耐熱性を有するものとされてい
る。この高温超純水製造装置によると、蒸発器(22)で得
られた75℃の高温超純水は、高温のままイオン交換装
置(26)の耐熱性混床式イオン交換樹脂または耐熱性強酸
性陽イオン交換樹脂に通される。これにより、高温超純
水中の金属イオンが極微量となるまで除去され、表3に
示す生産水熱交換器出口の高温超純水水質分析結果と同
等の75℃の高温超純水が得られる。
FIG. 2 shows a second embodiment of the apparatus for producing high-temperature ultrapure water according to the present invention. This high-temperature ultrapure water production system is the first
The difference from the embodiment is that the two heat exchangers (24) and (25) are both omitted, and accordingly, the mixed-bed ion exchange resin or the mixed bed ion exchange resin filled in the ion exchange device (26) is used. Strongly acidic cation exchange resins are said to have heat resistance. According to this high-temperature ultrapure water production apparatus, the high-temperature ultrapure water at 75 ° C. obtained by the evaporator (22) is kept at a high temperature without using the heat-resistant mixed-bed ion exchange resin or the heat-resistant strong acid of the ion exchange apparatus (26). Through a cation exchange resin. As a result, the metal ions in the high-temperature ultrapure water are removed to a very small amount, and the high-temperature ultrapure water at 75 ° C. equivalent to the analysis result of the high-temperature ultrapure water at the outlet of the production water heat exchanger shown in Table 3 is obtained. Can be

【0057】本発明の高温超純水製造装置で製造される
高温超純水は、低溶存酸素濃度でありかつ微量金属イオ
ンも除去されているので処理液を洗い流すためのリンス
水としてだけでなく、Si表面の自然酸化膜抑制やエッ
チング、あるいは自然酸化膜表面の金属不純物の除去を
目的とした薬液としても使用することができる。この場
合、本発明の高温超純水製造装置で製造される高温超純
水をプロセス装置に直接供給することになる。
The high-temperature ultrapure water produced by the apparatus for producing high-temperature ultrapure water of the present invention has a low dissolved oxygen concentration and also removes trace metal ions. Also, it can be used as a chemical solution for the purpose of suppressing or etching a natural oxide film on the Si surface or removing metal impurities on the surface of the natural oxide film. In this case, the high-temperature ultrapure water produced by the high-temperature ultrapure water production apparatus of the present invention is directly supplied to the process apparatus.

【0058】本発明の高温超純水製造装置で製造される
高温超純水を薬液として適用する場合の薬液調製装置の
実施例について、次に述べる。
Next, an embodiment of a chemical liquid preparation apparatus in the case where high-temperature ultrapure water produced by the high-temperature ultrapure water production apparatus of the present invention is applied as a chemical will be described.

【0059】図9は、本発明の薬液調製装置の第1実施
例を示している。同図に示すように、この薬液調製装置
は、本発明の高温超純水製造装置(31)と、高温超純水製
造装置(31)で製造される高温超純水を高温のまま通水し
て高温の電解イオン水を製造する電解イオン水製造装置
(32)とを備えている。電解イオン水製造装置(32)は、ア
ノード極(43)とカソード極(44)との間に、相対するイオ
ン交換膜(45)とこれらの間に充填されたイオン交換樹脂
(46)とが挟まれているもので、本発明の高温超純水製造
装置(31)で製造される高温超純水を高温のまま電解イオ
ン水製造装置(32)に通水することにより、高温の電解イ
オン水(電解アノード水と電解カソード水)が得られ
る。そして、電解アノード水が第1の循環ポンプ(36)付
き薬液槽(33)に供給され、電解カソード水が第2の循環
ポンプ(36)付き薬液槽(34)に供給され、高温超純水が超
純水リンス槽(35)に供給されている。
FIG. 9 shows a first embodiment of the chemical liquid preparation apparatus of the present invention. As shown in the figure, this chemical solution preparation apparatus is a high-temperature ultrapure water production apparatus (31) of the present invention and a high-temperature ultrapure water produced by a high-temperature ultrapure water production apparatus (31). Ionic water production equipment that produces high temperature electrolytic ionic water
(32). An electrolytic ionized water production device (32) is provided between an anode (43) and a cathode (44), an opposite ion exchange membrane (45) and an ion exchange resin filled between them.
(46) is sandwiched, and the high-temperature ultrapure water produced by the high-temperature ultrapure water production apparatus (31) of the present invention is passed through the electrolytic ionic water production apparatus (32) at a high temperature. Thus, high-temperature electrolytic ion water (electrolytic anode water and electrolytic cathode water) is obtained. Then, the electrolytic anode water is supplied to a chemical tank (33) with a first circulation pump (36), and the electrolytic cathode water is supplied to a chemical tank (34) with a second circulation pump (36). Is supplied to the ultrapure water rinsing tank (35).

【0060】図10は、本発明の薬液調製装置の第2実
施例を示している。同図に示すように、この薬液調製装
置は、本発明の高温超純水製造装置(31)と、高温超純水
製造装置(31)で製造される高温超純水を一定量の流量で
供給する高温超純水定量供給装置(37)と、薬液原液を一
定の流量で供給する自動薬液原液供給装置(38)と、高温
超純水と薬液原液を混合するミキサー(39)と、所望の濃
度となった薬液を所望の温度に昇温または冷却する温度
調節用熱交換器(40)とよりなる。
FIG. 10 shows a second embodiment of the chemical solution preparation apparatus of the present invention. As shown in the figure, this chemical solution preparation apparatus is a high-temperature ultrapure water production apparatus (31) of the present invention and a high-temperature ultrapure water produced by the high-temperature ultrapure water production apparatus (31) at a constant flow rate. A high-temperature ultrapure water quantitative supply device (37), an automatic undiluted chemical solution supply device (38) for supplying the undiluted chemical solution at a constant flow rate, a mixer (39) for mixing the high-temperature ultrapure water and the undiluted chemical solution, and And a temperature-regulating heat exchanger (40) for raising or cooling the chemical solution having the above concentration to a desired temperature.

【0061】高温超純水製造装置(31)で製造された高温
超純水と薬液原液とは、それぞれ高温超純水定量供給装
置(37)と自動薬液原液供給装置(38)で所望の濃度となる
ような比率の流量でミキサー(39)の前流に供給され、ミ
キサー(39)で完全に混合される。ミキサー(39)として
は、所望の濃度に調整された薬液の特別の供給装置を設
けずに済むラインミキサーが好ましいが、貯液槽に撹拌
機とポンプを備えたものでも良い。貯液槽からの薬液供
給方法としては、窒素ガスによる圧送方式でも良い。所
望の濃度に調整された薬液は、ミキサー(39)後流に設け
てある温度調節用熱交換器(40)により所望の温度に調節
される。所望の濃度に調整された薬液が所望の温度より
低い場合、温度調節用熱交換器(40)で昇温され、所望の
濃度に調整された薬液が所望の温度より高い場合、温度
調節用熱交換器(40)で冷却される。昇温する方法として
は、他に電気加熱あるいは蒸気加熱の方法がある。冷却
する方法としては、他に冷却塔あるいはチラー装置の冷
水を用いる方法がる。所望の濃度かつ所望の温度に調整
された薬液は、洗浄装置(41)の循環ポンプ(36)付き薬液
槽(42)に一定流量で連続して供給される。高温超純水は
超純水リンス槽(35)に供給される。薬液槽(42)の薬液
は、循環ポンプ(36)吐出側より供給量と同じ量が連続し
て抜き出される。薬液槽(42)への薬液の供給量は、ウエ
ハの処理量あるいはウエハ処理量に対応する汚染物質の
薬液槽(42)内濃度に対する製品の歩留まりの関係より決
定される。
The high-temperature ultrapure water and the undiluted chemical solution produced by the high-temperature ultrapure water production unit (31) are respectively subjected to the desired concentration by the high-temperature ultrapure water quantitative supply unit (37) and the automatic undiluted chemical liquid supply unit (38). The mixture is supplied to the upstream side of the mixer (39) at such a flow rate as to be obtained, and is completely mixed by the mixer (39). As the mixer (39), a line mixer which does not require a special supply device for a chemical solution adjusted to a desired concentration is preferable, but a mixer provided with a stirrer and a pump in a liquid storage tank may be used. As a method of supplying the chemical solution from the liquid storage tank, a pressure feeding method using nitrogen gas may be used. The chemical solution adjusted to a desired concentration is adjusted to a desired temperature by a temperature adjusting heat exchanger (40) provided downstream of the mixer (39). When the chemical solution adjusted to the desired concentration is lower than the desired temperature, the temperature is raised in the temperature adjusting heat exchanger (40), and when the chemical solution adjusted to the desired concentration is higher than the desired temperature, the temperature adjusting heat exchanger is used. Cooled in the exchanger (40). As a method for raising the temperature, there are other methods such as electric heating or steam heating. As another cooling method, there is a method using cold water of a cooling tower or a chiller device. The chemical solution adjusted to a desired concentration and a desired temperature is continuously supplied at a constant flow rate to a chemical solution tank (42) with a circulation pump (36) of the cleaning device (41). The high-temperature ultrapure water is supplied to an ultrapure water rinsing tank (35). The chemical liquid in the chemical liquid tank (42) is continuously extracted from the discharge side of the circulation pump (36) in the same amount as the supply amount. The supply amount of the chemical solution to the chemical solution tank (42) is determined based on the relationship between the processing amount of the wafer or the product yield with respect to the concentration of the contaminant in the chemical solution tank (42) corresponding to the wafer processing amount.

【0062】図11は、本発明の薬液調製装置の第3実
施例を示している。この薬液調製装置が第2実施例と異
なる点は、同図に示すように、温度調節用熱交換器(40)
が省略されている点である。この装置によると、高温超
純水製造装置(31)で製造された高温超純水と薬液原液と
が、それぞれ高温超純水定量供給装置(37)と自動薬液原
液供給装置(38)で所望の濃度となるような比率の流量で
ミキサー(39)の前流に供給され、ミキサー(39)で完全に
混合されて、所望の温度とされる。第2実施例と同じ構
成のものについては、同じ符号を付して説明を省略す
る。
FIG. 11 shows a third embodiment of the chemical liquid preparation apparatus according to the present invention. The difference between this chemical solution preparation apparatus and the second embodiment is that, as shown in FIG.
Is omitted. According to this apparatus, the high-temperature ultrapure water and the undiluted chemical solution produced by the high-temperature ultrapure water production unit (31) are respectively desired by the high-temperature ultrapure water quantitative supply unit (37) and the automatic undiluted chemical solution supply unit (38). The mixture is supplied to the upstream of the mixer (39) at a flow rate such that the concentration becomes as described above, and is thoroughly mixed by the mixer (39) to reach a desired temperature. Components having the same configuration as the second embodiment are denoted by the same reference numerals, and description thereof is omitted.

【0063】図12は、本発明の薬液調製装置の第4実
施例を示している。同図に示すように、この薬液調製装
置には、ミキサー(39)が設けられておらず、本発明の高
温超純水製造装置(31)で製造された高温超純水と薬液原
液とが、それぞれ高温超純水定量供給装置(37)と自動薬
液原液供給装置(38)で所望の濃度となるような比率の流
量で洗浄装置(41)の循環ポンプ(36)付き薬液槽(42)に直
接供給されるものである。
FIG. 12 shows a fourth embodiment of the chemical solution preparation apparatus according to the present invention. As shown in the figure, the chemical solution preparation device is not provided with a mixer (39), and the high temperature ultrapure water and the drug solution stock solution produced by the high temperature ultrapure water production device (31) of the present invention are used. A chemical solution tank (42) with a circulation pump (36) of a cleaning device (41) at a flow rate such that the desired concentration is obtained by a high-temperature ultrapure water fixed-quantity supply device (37) and an automatic chemical solution supply device (38), respectively. Are supplied directly to

【0064】なお、本発明の薬液調製装置において、高
温超純水に混合される薬剤は、薬液原液に限られるもの
ではなく、例えば、半導体製造工程でのウエハ洗浄に用
いられる薬品のうち、ガスの状態で貯蔵・供給される材
料ガスや酸化系ガスを、本発明の高温超純水製造装置(3
1)で製造された高温超純水に直接ガスの状態で所望の濃
度となる比率で吹き込み・混合して、所望の温度として
供給しても良い。
In the chemical liquid preparation apparatus of the present invention, the chemical mixed with the high-temperature ultrapure water is not limited to the chemical liquid stock solution. The raw material gas and the oxidizing gas stored and supplied in the state of
The high-temperature ultrapure water produced in 1) may be directly blown and mixed in a ratio of a desired concentration in a gaseous state, and supplied at a desired temperature.

【0065】[0065]

【発明の効果】本発明の高温超純水製造装置によると、
前処理系で処理された前処理水、あるいは、一次純水系
で処理された一次純水に含まれているシリカや有機物な
どの非イオン性不純物および溶存酸素が、蒸発器によっ
て除去される。また、蒸発器は100℃程度の高温で操
作されるので、生菌がなくバクテリアの殺菌が不要であ
る。蒸発器に金属イオン溶出防止処理が施されていない
場合、蒸発器で得られた高温超純水には、微量の金属イ
オンが含まれることになるが、この微量金属イオンは、
イオン交換装置に通されることにより除去され、半導体
製造工程のウエハ洗浄に用いられても問題ないレベルの
高温超純水が得られる。
According to the high-temperature ultrapure water production apparatus of the present invention,
Non-ionic impurities such as silica and organic substances and dissolved oxygen contained in the pretreatment water treated in the pretreatment system or the primary pure water treated in the primary pure water system are removed by the evaporator. Further, since the evaporator is operated at a high temperature of about 100 ° C., there is no viable bacteria and sterilization of bacteria is not required. If the evaporator has not been subjected to metal ion elution prevention treatment, high-temperature ultrapure water obtained in the evaporator will contain a trace amount of metal ions, but this trace amount of metal ions,
It is removed by passing through an ion exchange device, and high-temperature ultrapure water at a level that does not cause any problem even when used for cleaning a wafer in a semiconductor manufacturing process is obtained.

【0066】本発明の高温超純水製造装置は、紫外線殺
菌装置、デミネライザーおよび限外濾過装置よりなる2
次純水系を備えた従来例1の装置と比較して、装置の構
成が単純で、運転監視、維持管理が楽である。しかも、
金属イオン溶出防止処理すなわち電解複合研磨および高
温炉での強制酸化皮膜処理を蒸発器に施さなくてもよい
ので、従来例2の装置と比較して、装置の製造工程が簡
略化され、製造コストが低減できる。
The high-temperature ultrapure water production apparatus of the present invention comprises an ultraviolet sterilizer, a demineralizer and an ultrafiltration apparatus.
Compared with the device of the first conventional example provided with a secondary pure water system, the configuration of the device is simple, and operation monitoring and maintenance are easy. Moreover,
Since the metal ion elution prevention treatment, that is, the electrolytic combined polishing and the forced oxide film treatment in the high-temperature furnace do not need to be performed on the evaporator, the manufacturing process of the device is simplified as compared with the device of the conventional example 2, and the manufacturing cost is reduced. Can be reduced.

【0067】さらに、蒸発器で得られる純水は、金属
(Fe、Ni)イオンを極微量例えばFe50ppt、
Ni10ppt程度含む以外は半導体製造工程のウエハ
洗浄に使用される超純水の水質と同等、あるいはそれ以
上の水質を有しているから、これを処理する混床式イオ
ン交換樹脂または強酸性陽イオン交換樹脂の寿命が非常
に長くなり、ランニングコストが増加することなく、半
導体製造工程のウエハ洗浄に使用されても問題ないレベ
ルの高温超純水を製造することができる。
Further, the pure water obtained by the evaporator contains a very small amount of metal (Fe, Ni) ions, for example, Fe 50 ppt,
Except for containing about 10 ppt of Ni, it has water quality equal to or higher than that of ultrapure water used for cleaning wafers in the semiconductor manufacturing process. It is possible to produce high-temperature ultrapure water at a level that does not cause any problem even when used for cleaning a wafer in a semiconductor manufacturing process, without prolonging the life of the exchange resin and increasing running costs.

【0068】蒸発器で得られた高温の微量金属イオン未
除去超純水とイオン交換装置で処理された常温の微量金
属イオン除去済み超純水とを熱交換する生産水熱交換器
をさらに備えているものでは、イオン交換装置に充填さ
れる混床式イオン交換樹脂および強酸性陽イオン交換樹
脂は、耐熱性をそれほど有していないものでよく、ま
た、生産水熱交換器により熱回収が行われるので、熱損
失を抑えることができる。
A production water heat exchanger for heat-exchanging high-temperature trace metal ion-free ultrapure water obtained by the evaporator and ultra-temperature-free trace metal ion-free ultrapure water treated by the ion exchanger is further provided. However, the mixed-bed ion exchange resin and the strongly acidic cation exchange resin that are filled in the ion exchange device may not have much heat resistance, and heat recovery may be performed by a production water heat exchanger. As a result, heat loss can be suppressed.

【0069】また、生産水熱交換器で冷却された微量金
属イオン未除去超純水を40℃以下まで冷却してイオン
交換装置への供給水とする冷却熱交換器をさらに備えて
いるものでは、イオン交換装置に入る前の超純水を所定
温度以下に確実に冷却することができる。
Further, there is further provided a cooling heat exchanger which cools ultrapure water from which trace metal ions have not been removed cooled by the production water heat exchanger to 40 ° C. or lower to supply water to the ion exchange apparatus. In addition, ultrapure water before entering the ion exchange device can be reliably cooled to a predetermined temperature or lower.

【0070】さらに、イオン交換装置が連続通水型電気
脱イオン装置であるものでは、イオン交換樹脂の再生の
ための装置運転停止が必要なく、完全な連続運転が可能
となる。
Further, in the case where the ion exchange device is a continuous water passing type electrodeionization device, the device operation for regeneration of the ion exchange resin does not need to be stopped, and complete continuous operation is possible.

【0071】生産水熱交換器をチタン製、電解研磨・特
殊熱処理をした酸化不動態ステンレス鋼製または電解複
合研磨・特殊熱処理をした酸化不動態ステンレス鋼製と
し、冷却熱交換器をステンレス鋼製としたものでは、ス
テンレス鋼製熱交換器から金属イオンが極微量溶出した
場合、この微量金属イオンがイオン交換装置で除去さ
れ、その後、微量金属イオン除去済み超純水は、溶出が
ほとんど無い生産水熱交換器により加熱されるので、最
終的に得られる高温の超純水の水質が悪くなることはな
い。また、金属材料を用いた熱交換器は、従来の超純水
の熱交換器に使用されているPFAやPVDF等のふっ
素樹脂で製作された熱交換器に比べ、熱伝達率が大きく
加工が容易であるので、コンパクトで安価なものにでき
るという利点も有している。
The production water heat exchanger is made of titanium, oxidation-passive stainless steel subjected to electrolytic polishing and special heat treatment, or oxidation-passive stainless steel subjected to electrolytic combined polishing and special heat treatment, and the cooling heat exchanger is made of stainless steel. When very small amounts of metal ions are eluted from the stainless steel heat exchanger, the trace metal ions are removed by the ion exchange device, and then ultrapure water from which trace metal ions have been removed is produced with little elution Since the water is heated by the water heat exchanger, the quality of the finally obtained high-temperature ultrapure water does not deteriorate. In addition, heat exchangers using metal materials have a higher heat transfer coefficient than conventional heat exchangers made of fluororesins such as PFA and PVDF, which are used for heat exchangers of ultrapure water. Because it is easy, it also has the advantage of being compact and inexpensive.

【0072】高温超純水製造装置と、高温超純水製造装
置により得られた高温超純水を電解アノード水と電解カ
ソード水とに分解する電界イオン水製造装置と、電解ア
ノード水および電解カソード水を直接半導体もしくはそ
の他の精密デバイスの処理装置の薬液槽に供給する供給
装置とを備えている薬液調製装置によると、常温に比べ
て洗浄性がよくなる高温の電解イオン水が得られるの
で、洗浄時間を短縮できるとともに、薬液の使用料を削
減できる。
A high-temperature ultrapure water producing apparatus, an electric field ion water producing apparatus for decomposing high-temperature ultrapure water obtained by the high-temperature ultrapure water producing apparatus into an electrolytic anode water and an electrolytic cathode water, an electrolytic anode water and an electrolytic cathode According to a chemical solution preparation device having a supply device for directly supplying water to a chemical solution tank of a processing device of a semiconductor or other precision device, high-temperature electrolytic ionic water that can be easily cleaned compared to room temperature can be obtained. The time can be shortened and the fee for using the chemical can be reduced.

【0073】また、本発明の薬液調製装置により得られ
た薬液を薬液槽に供給する方法として、所望の濃度でか
つ所望の温度とした薬液を所定量で連続して薬液槽に供
給するとともに、供給量と同等の量を薬液槽から抜き出
す方法を用いた場合、薬液槽の性状が一定となり、した
がって、薬液の性状変化による製品のバラツキが少なく
なり歩留まりが向上する。さらに、連続運転が可能であ
るので、洗浄停止時間がなくなり、バッチ方式に比べ稼
働時間が増えて生産性が高くなる。
Further, as a method for supplying the chemical solution obtained by the chemical solution preparation device of the present invention to the chemical solution tank, a predetermined amount of the chemical solution having a desired concentration and a desired temperature is continuously supplied to the chemical solution tank. When a method of extracting an amount equivalent to the supply amount from the chemical solution tank is used, the properties of the chemical solution tank become constant, and therefore, variations in products due to changes in the properties of the chemical solution are reduced, and the yield is improved. Further, since the continuous operation is possible, the cleaning stop time is eliminated, and the operation time is increased as compared with the batch method, so that the productivity is increased.

【0074】なお、所望の濃度でかつ所望の温度とした
薬液を薬液槽にバッチ方式で供給する方法でも、供給す
る純水が高温超純水なので従来の室温の超純水供給に比
べ、所望の温度にするための昇温時間が短縮できる。
Even in a method of supplying a chemical solution having a desired concentration and a desired temperature to a chemical solution tank in a batch system, since pure water to be supplied is high-temperature ultrapure water, compared with the conventional ultrapure water supply at room temperature, it is more desirable. The time required for raising the temperature can be shortened.

【図面の簡単な説明】[Brief description of the drawings]

【図1】この発明の高温超純水製造装置の第1実施例を
示すフローシートである。
FIG. 1 is a flow sheet showing a first embodiment of a high-temperature ultrapure water production apparatus of the present invention.

【図2】この発明の高温超純水製造装置の第2実施例を
示すフローシートである。
FIG. 2 is a flow sheet showing a second embodiment of the high-temperature ultrapure water production apparatus of the present invention.

【図3】従来の超純水製造装置を示すフローシートであ
る。
FIG. 3 is a flow sheet showing a conventional ultrapure water production apparatus.

【図4】従来の高温超純水製造装置を示すフローシート
である。
FIG. 4 is a flow sheet showing a conventional high-temperature ultrapure water production apparatus.

【図5】半導体プロセスの処理工程の例を示す図であ
る。
FIG. 5 is a diagram illustrating an example of a processing step of a semiconductor process.

【図6】連続通水型電気脱イオン装置の1例を示す図で
ある。
FIG. 6 is a diagram showing an example of a continuous water flow type electrodeionization apparatus.

【図7】連続通水型電気脱イオン装置の他の例を示す図
である。
FIG. 7 is a view showing another example of a continuous water flow type electrodeionization apparatus.

【図8】連続通水型電気脱イオン装置のさらに他の例を
示す図である。
FIG. 8 is a view showing still another example of the continuous water flow type electrodeionization apparatus.

【図9】この発明の薬液調製装置の第1実施例を示すフ
ローシートである。
FIG. 9 is a flow sheet showing a first embodiment of the drug solution preparation device of the present invention.

【図10】この発明の薬液調製装置の第2実施例を示す
フローシートである。
FIG. 10 is a flow sheet showing a second embodiment of the drug solution preparation device of the present invention.

【図11】この発明の薬液調製装置の第3実施例を示す
フローシートである。
FIG. 11 is a flow sheet showing a third embodiment of the drug solution preparation device of the present invention.

【図12】この発明の薬液調製装置の第4実施例を示す
フローシートである。
FIG. 12 is a flow sheet showing a fourth embodiment of the drug solution preparation device of the present invention.

【符号の説明】[Explanation of symbols]

21:一次純水系 22:多重効用蒸発器 23:イオン交換装置 24:生産水熱交換器 25:冷却熱交換器 26:イオン交換装置 31:高温超純水製造装置 32:電界イオン水製造装置 39:ミキサー(混合装置) 21: Primary pure water system 22: Multiple effect evaporator 23: Ion exchange device 24: Production water heat exchanger 25: Cooling heat exchanger 26: Ion exchange device 31: High temperature ultrapure water production device 32: Electric field ion water production device 39 : Mixer (mixing device)

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 FI C02F 9/00 503 C02F 9/00 503B 504 504B 1/46 1/46 A H01L 21/304 341 H01L 21/304 341Z (72)発明者 木場 和則 大阪市此花区西九条5丁目3番28号 日立 造船株式会社内 (72)発明者 百瀬 祥一 大阪市此花区西九条5丁目3番28号 日立 造船株式会社内 (72)発明者 岩井 俊憲 大阪市此花区西九条5丁目3番28号 日立 造船株式会社内──────────────────────────────────────────────────の Continuation of front page (51) Int.Cl. 6 Identification code FI C02F 9/00 503 C02F 9/00 503B 504 504B 1/46 1/46 A H01L 21/304 341 H01L 21/304 341Z (72) Inventor Kazunori Kiba 5-3-28 Nishikujo, Konohana-ku, Osaka City Inside Hitachi Zosen Corporation (72) Inventor Shoichi Momose 5-28 Nishikujo, Konohana-ku, Osaka City Inside Hitachi Zosen Corporation (72) Invention Person Toshinori Iwai 5-3-28 Nishikujo, Konohana-ku, Osaka Inside Hitachi Zosen Corporation

Claims (19)

【特許請求の範囲】[Claims] 【請求項1】 原水を凝集ろ過し脱気処理した前処理
水、あるいは、一次純水系で得られた一次純水を処理し
て高温の超純水を得る蒸発器と、蒸発器で得られた超純
水に含まれる微量金属イオンを除去するイオン交換装置
とを備えている高温超純水製造装置。
1. An evaporator that obtains high-temperature ultrapure water by treating pretreated water obtained by subjecting raw water to coagulation filtration and degassing, or primary water obtained by a primary pure water system, and an evaporator. A high-temperature ultrapure water production apparatus, comprising: an ion exchange apparatus for removing trace metal ions contained in the ultrapure water.
【請求項2】 イオン交換装置が、混床式イオン交換樹
脂または強酸性陽イオン交換樹脂を充填している請求項
1の高温超純水製造装置。
2. The high temperature ultrapure water production apparatus according to claim 1, wherein the ion exchange apparatus is filled with a mixed bed type ion exchange resin or a strongly acidic cation exchange resin.
【請求項3】 イオン交換装置が、イオン交換膜または
イオン交換繊維を充填している請求項1の高温超純水製
造装置。
3. The high-temperature ultrapure water production apparatus according to claim 1, wherein the ion exchange apparatus is filled with an ion exchange membrane or ion exchange fibers.
【請求項4】 イオン交換装置が、連続通水型電気脱イ
オン交換装置である請求項1の高温超純水製造装置。
4. The high-temperature ultrapure water production apparatus according to claim 1, wherein the ion exchange apparatus is a continuous water-flow type electrodeionization apparatus.
【請求項5】 イオン交換装置が、耐熱性の混床式イオ
ン交換樹脂、耐熱性の強酸性陽イオン交換樹脂、耐熱性
のイオン交換膜または耐熱性のイオン交換繊維を充填し
ている請求項1の高温超純水製造装置。
5. The ion exchange apparatus is filled with a heat-resistant mixed-bed ion-exchange resin, a heat-resistant strongly acidic cation-exchange resin, a heat-resistant ion exchange membrane, or a heat-resistant ion exchange fiber. 1. High temperature ultrapure water production equipment.
【請求項6】 蒸発器で得られた高温の微量金属イオン
未除去超純水とイオン交換装置で処理された常温の微量
金属イオン除去済み超純水とを熱交換することにより、
上記高温の微量金属イオン未除去超純水をイオン交換装
置への供給前に冷却するとともに、常温の微量金属イオ
ン除去済み超純水を加熱する生産水熱交換器をさらに備
えている請求項1から4の高温超純水製造装置。
6. Heat exchange between the high-temperature trace metal ion-free ultrapure water obtained in the evaporator and the room temperature trace metal ion-free ultrapure water treated by the ion exchanger.
2. A production water heat exchanger for cooling the high-temperature ultrapure water from which trace metal ions have not been removed before supplying the ultrapure water to the ion exchanger, and heating the ultrapure water from which trace metal ions have been removed at room temperature. To 4 high-temperature ultrapure water production equipment.
【請求項7】 生産水熱交換器で冷却された微量金属イ
オン未除去超純水を40℃以下まで冷却してイオン交換
装置への供給水とする冷却熱交換器をさらに備えている
請求項6の高温超純水製造装置。
7. A cooling heat exchanger further comprising cooling the ultrapure water from which trace metal ions have not been removed cooled by the production water heat exchanger to 40 ° C. or less to supply water to the ion exchange device. 6. High temperature ultrapure water production equipment.
【請求項8】 生産水熱交換器の接液部が、チタン製、
電解研磨に特殊熱処理をした酸化不動態ステンレス鋼製
または電解複合研磨に特殊熱処理をした酸化不動態ステ
ンレス鋼製である請求項6または7の高温超純水製造装
置。
8. The production water heat exchanger, wherein the liquid contact portion is made of titanium;
8. The high-temperature ultrapure water production apparatus according to claim 6, wherein the apparatus is made of an oxidation-passive stainless steel subjected to a special heat treatment for electrolytic polishing or an oxidation-passive stainless steel subjected to a special heat treatment for electrolytic combined polishing.
【請求項9】 冷却熱交換器の接液部が、ステンレス鋼
製、チタン製、電解研磨に特殊熱処理をした酸化不動態
ステンレス鋼製または電解複合研磨に特殊熱処理をした
酸化不動態ステンレス鋼製である請求項7の高温超純水
製造装置。
9. The liquid contact part of the cooling heat exchanger is made of stainless steel, titanium, oxidation passivated stainless steel subjected to special heat treatment for electrolytic polishing, or oxidation passivated stainless steel subjected to special heat treatment for electrolytic combined polishing. The high-temperature ultrapure water production apparatus according to claim 7, wherein
【請求項10】 請求項1から9の高温超純水製造装置
と、高温超純水製造装置により得られた高温超純水を電
解アノード水と電解カソード水とに分解する電界イオン
水製造装置と、電解アノード水および電解カソード水を
直接半導体もしくはその他の精密デバイスの処理装置の
薬液槽に供給する供給装置とを備えている薬液調製装
置。
10. A high-temperature ultrapure water production apparatus according to claim 1, and an electric field ion water production apparatus for decomposing the high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus into electrolytic anode water and electrolytic cathode water. And a supply device for directly supplying an electrolytic anode water and an electrolytic cathode water to a chemical tank of a semiconductor or other precision device processing apparatus.
【請求項11】 請求項1から9の高温超純水製造装置
と、高温超純水製造装置により得られた高温超純水およ
び高温超純水に混合される薬剤を半導体もしくはその他
の精密デバイスの処理装置の薬液槽に直接供給するとと
もに、薬液槽内の薬液が所望の温度あるいは濃度となる
ように調整する薬液供給調整装置とを備えている薬液調
製装置。
11. A high-temperature ultrapure water production apparatus according to claim 1, wherein the high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus and a drug mixed with the high-temperature ultrapure water are used as a semiconductor or other precision device. And a chemical solution supply adjusting device for directly supplying the chemical solution in the chemical solution tank to a desired temperature or concentration and for directly supplying the chemical solution in the chemical solution tank.
【請求項12】 請求項1から9の高温超純水製造装置
と、高温超純水製造装置により得られた高温超純水に薬
剤を混合して、半導体もしくはその他の精密デバイスの
処理装置の薬液槽に供給される薬液を得る混合装置とを
備えている薬液調製装置。
12. A high-temperature ultrapure water production apparatus according to claim 1 and a high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus, wherein a chemical is mixed with the high-temperature ultrapure water to obtain a semiconductor or other precision device processing apparatus. A mixing device for obtaining a chemical solution supplied to the chemical solution tank.
【請求項13】 請求項1から9の高温超純水製造装置
と、高温超純水製造装置により得られた高温超純水に、
HCl、NH3 、HF、NH4 F、SOx、NOx等の
材料ガスやO3 、O2 、酸素ラジカルなどの酸化系ガス
を混合する混合装置とを備えている薬液調製装置。
13. The high-temperature ultrapure water production apparatus according to claim 1 and the high-temperature ultrapure water obtained by the high-temperature ultrapure water production apparatus,
A chemical liquid preparation device including a mixing device for mixing a material gas such as HCl, NH 3 , HF, NH 4 F, SOx, and NOx and an oxidizing gas such as O 3 , O 2 , and oxygen radicals.
【請求項14】 請求項1から9の高温超純水製造装置
を用いて高温超純水を得る高温超純水製造方法。
14. A method for producing high-temperature ultrapure water using the high-temperature ultrapure water production apparatus according to claim 1.
【請求項15】 請求項10から13の薬液調製装置を
用いて半導体もしくはその他の精密デバイスの製造に使
用される薬液を得る薬液調製方法。
15. A chemical liquid preparation method for obtaining a chemical liquid used in the manufacture of semiconductors or other precision devices using the chemical liquid preparation apparatus according to claim 10.
【請求項16】 請求項14の方法により得られた高温
超純水。
16. High-temperature ultrapure water obtained by the method of claim 14.
【請求項17】 請求項15の方法により得られた薬
液。
17. A chemical obtained by the method according to claim 15.
【請求項18】 請求項16の高温超純水によって洗浄
された半導体もしくはその他の精密デバイス。
18. A semiconductor or other precision device cleaned by the high-temperature ultrapure water according to claim 16.
【請求項19】 請求項17の薬液によって処理されか
つ請求項16の高温超純水によって洗浄された半導体も
しくはその他の精密デバイス。
19. A semiconductor or other precision device treated with the chemical solution of claim 17 and washed with the high-temperature ultrapure water of claim 16.
JP9079277A 1997-03-31 1997-03-31 High-temperature ultrapure water production apparatus and chemical liquid preparation apparatus equipped with the same Pending JPH10272492A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP9079277A JPH10272492A (en) 1997-03-31 1997-03-31 High-temperature ultrapure water production apparatus and chemical liquid preparation apparatus equipped with the same
CNB988112922A CN1163418C (en) 1997-03-31 1998-09-18 High-temperature ultrahigh-purity water production equipment
PCT/JP1998/004214 WO2000017108A1 (en) 1997-03-31 1998-09-18 High temperature ultra-pure water production apparatus and liquid medicine preparation apparatus equipped with the production apparatus
US09/554,558 US6562205B1 (en) 1997-03-31 1998-09-18 High-temperature ultrapure water production apparatus and liquid medicine preparation apparatus equipped with the production apparatus
TW087115916A TW514626B (en) 1997-03-31 1998-09-24 Apparatus for manufacturing high-temperature extra-pure water and chemical processing apparatus having the same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP9079277A JPH10272492A (en) 1997-03-31 1997-03-31 High-temperature ultrapure water production apparatus and chemical liquid preparation apparatus equipped with the same
PCT/JP1998/004214 WO2000017108A1 (en) 1997-03-31 1998-09-18 High temperature ultra-pure water production apparatus and liquid medicine preparation apparatus equipped with the production apparatus

Publications (1)

Publication Number Publication Date
JPH10272492A true JPH10272492A (en) 1998-10-13

Family

ID=26420309

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9079277A Pending JPH10272492A (en) 1997-03-31 1997-03-31 High-temperature ultrapure water production apparatus and chemical liquid preparation apparatus equipped with the same

Country Status (3)

Country Link
JP (1) JPH10272492A (en)
CN (1) CN1163418C (en)
WO (1) WO2000017108A1 (en)

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