JP2010123897A - Startup cleaning method for warm ultrapure water supply use-point piping - Google Patents
Startup cleaning method for warm ultrapure water supply use-point piping Download PDFInfo
- Publication number
- JP2010123897A JP2010123897A JP2008298635A JP2008298635A JP2010123897A JP 2010123897 A JP2010123897 A JP 2010123897A JP 2008298635 A JP2008298635 A JP 2008298635A JP 2008298635 A JP2008298635 A JP 2008298635A JP 2010123897 A JP2010123897 A JP 2010123897A
- Authority
- JP
- Japan
- Prior art keywords
- ultrapure water
- cleaning
- water
- temperature
- use point
- 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.)
- Granted
Links
- 239000012498 ultrapure water Substances 0.000 title claims abstract description 104
- 229910021642 ultra pure water Inorganic materials 0.000 title claims abstract description 103
- 238000004140 cleaning Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 claims description 28
- 239000002033 PVDF binder Substances 0.000 claims description 18
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 18
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 17
- 239000008213 purified water Substances 0.000 abstract description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 21
- 229910052731 fluorine Inorganic materials 0.000 description 21
- 239000011737 fluorine Substances 0.000 description 21
- 238000010828 elution Methods 0.000 description 18
- 239000004065 semiconductor Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000011109 contamination Methods 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Images
Landscapes
- Cleaning In General (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
本発明は、半導体デバイス、液晶ディスプレイ、シリコンウェハ、プリント基板等の電子部品製造工場、原子力発電所又は医薬品製造工場等で広く利用される超純水を製造供給する超純水製造装置の立上洗浄方法に関し、特に超純水を加温して温超純水としてユースポイントへ供給する温超純水製造装置のユースポイント配管の立上洗浄方法に関する。 The present invention establishes an ultrapure water production apparatus for producing and supplying ultrapure water widely used in electronic component manufacturing factories such as semiconductor devices, liquid crystal displays, silicon wafers, printed circuit boards, nuclear power plants or pharmaceutical manufacturing factories. The present invention relates to a cleaning method, and more particularly to a method for standing-up cleaning of a point-of-use pipe of a warm ultrapure water production apparatus that heats ultrapure water and supplies it to a point of use as warm ultrapure water.
従来から、半導体デバイス等の半導体製造工程においては、物質、微粒子、有機物、溶存ガス及び生菌等の不純物含有量が極めて少ない超純水が使用されている。そして、半導体デバイスの集積度の向上にともなって、超純水の純度に対する要求は益々厳しくなってきている。 2. Description of the Related Art Conventionally, in a semiconductor manufacturing process such as a semiconductor device, ultrapure water having an extremely small content of impurities such as substances, fine particles, organic substances, dissolved gas and viable bacteria has been used. As the degree of integration of semiconductor devices increases, the demand for the purity of ultrapure water has become increasingly severe.
このような半導体製造における洗浄工程では、有機物汚染、パーティクル汚染、重金属汚染等の除去又は自然酸化膜の除去等を目的として、硫酸と過酸化水素水との混合液、アンモニア水と過酸化水素水との混合液、塩酸と過酸化水素水との混合液、又は希フッ酸水溶液等の洗浄薬液を用いて洗浄した後、これらの洗浄薬液を洗い流すために超純水で洗浄することが多い。このような洗浄薬液を用いた洗浄工程においては、超純水洗浄が不充分であれば、洗浄薬液に由来する硫酸基や硝酸基等がシリコンウェハの表面等に残り、半導体製品における不良発生の原因となってしまうことから、超純水洗浄による洗浄薬液の除去は完全になされなければならない。 In such a cleaning process in semiconductor manufacturing, a mixed solution of sulfuric acid and hydrogen peroxide solution, ammonia water and hydrogen peroxide solution for the purpose of removing organic matter contamination, particle contamination, heavy metal contamination, etc. or removing a natural oxide film, etc. After washing with a cleaning liquid such as a mixed liquid of hydrochloric acid and a hydrogen peroxide solution, or a dilute hydrofluoric acid aqueous solution, it is often washed with ultrapure water to wash away these cleaning liquids. In such a cleaning process using a cleaning chemical, if ultrapure water cleaning is insufficient, sulfuric acid groups and nitric acid groups derived from the cleaning chemical remain on the surface of the silicon wafer, etc. Therefore, the cleaning chemical solution must be completely removed by the ultrapure water cleaning.
ところで、水は、全ての物質をたとえわずかといえども溶解させる能力を有しており、この水の溶解能力は一般に温度が高くなるほど大きくなる。そこで、半導体製造における洗浄工程でも温超純水を用いるのが一般的である。 By the way, water has the ability to dissolve all substances, even if only a little, and the solubility ability of water generally increases as the temperature increases. Therefore, it is common to use warm ultrapure water in the cleaning process in semiconductor manufacturing.
このような温超純水により洗浄を行う場合、超純水を加熱して温超純水を得るための装置、すなわち純水加熱装置を半導体製造ラインに設置しておく必要がある。このような純水加熱装置においては、前述したように高温の超純水が全ての物質に対して溶解能力を有していることから、その溶解能力によって純水製造装置の構成材料が純水に溶出してしまい、その純水加熱装置を経て供給される温純水が逆に汚染源となってしまうおれがある。 When cleaning with such warm ultrapure water, it is necessary to install an apparatus for heating the ultrapure water to obtain warm ultrapure water, that is, a pure water heating apparatus, in the semiconductor production line. In such a pure water heating device, as described above, high-temperature ultrapure water has the ability to dissolve all substances, so that the constituent material of the pure water production device is purified water by the dissolving capability. The hot pure water supplied through the pure water heating device may be a source of contamination.
そこで、純水加熱装置をユースポイントの直前に配置して加熱後の温超純水をユースポイント配管によりユースポイントまで供給している。このようなユースポイント配管としては、耐熱性を有することが必要である。そこで、金属材料を用いることが考えられるが、その金属材料が金属汚染源となるおそれがあることから、金属材料を使用することは適当でない。このため、合成樹脂製配管が用いられているが、耐溶出性、耐熱性、経済性等の観点から、ポリフッ化ビニリデン（ＰＶＤＦ）、テトラフルオロエチレン−パーフルオロアルキルビニルエーテル共重合体（ＰＦＡ）、テトラフルオロエチレン−ヘキサフルオロプロピレン共重合体（ＦＥＰ）等のフッ素系樹脂を内面に配したものが使用されている。 Therefore, a pure water heating device is arranged immediately before the use point, and heated ultra pure water is supplied to the use point through the use point piping. Such a use point pipe needs to have heat resistance. Therefore, it is conceivable to use a metal material, but it is not appropriate to use a metal material because the metal material may become a metal contamination source. For this reason, synthetic resin piping is used, but from the viewpoints of elution resistance, heat resistance, economy, etc., polyvinylidene fluoride (PVDF), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), A material in which a fluororesin such as tetrafluoroethylene-hexafluoropropylene copolymer (FEP) is arranged on the inner surface is used.
前述のような半導体製造ラインの温超純水製造装置の新規立ち上げ時、又は定期検査等による休止後の再立ち上げ時には、系内に混入・発生する不純物を除去してユースポイントにおける超純水が所望の水質に至るまで洗浄試運転を行う。この場合、工場の稼働効率の向上を目的として、装置の立ち上げ期間（すなわち、試運転・調整期間）の短縮、いわゆる装置の垂直立ち上げと称される短期立ち上げが強く求められている。 When a new warm-up ultrapure water production system for a semiconductor production line as described above is started up, or when it is restarted after an outage due to periodic inspections, etc., impurities mixed and generated in the system are removed, and ultrapure water at the point of use is removed. A cleaning trial run is performed until the desired water quality is achieved. In this case, for the purpose of improving the operation efficiency of the factory, there is a strong demand for shortening the start-up period of the apparatus (that is, the trial operation / adjustment period), that is, so-called vertical start-up of the apparatus.
しかしながら、近年の高水質の要求から、系内の不純物を除去するとともに溶出物を抑制し、要求水質を満たすまで長期間を要することがあり、特に温超純水の場合には１月以上を要することもあり、温超純水製造装置における立ち上げ期間の短縮は急務であった。 However, due to the recent demand for high water quality, it may take a long time to remove impurities in the system and suppress the effluent, and to satisfy the required water quality, especially in the case of warm ultrapure water, it may take more than a month. There was also an urgent need to shorten the start-up period of the hot ultrapure water production system.
本発明は、上記課題に鑑みてなされたものであり、立ち上げ期間の短縮の可能な温超純水製造装置のユースポイント配管の立上洗浄方法を提供することを目的とする。 This invention is made | formed in view of the said subject, and it aims at providing the standing cleaning method of the use point piping of the warm ultrapure water manufacturing apparatus which can shorten a starting period.
上記課題を解決するために、本発明は、超純水を加温して温超純水としてユースポイントへ供給する温超純水製造装置のユースポイント配管の立ち上げ時の洗浄方法であって、供給する温超純水の水温よりも高い水温で前記ユースポイント配管の洗浄を行うことを特徴とする温超純水供給ユースポイント配管の立上洗浄方法を提供する（請求項１）。 In order to solve the above problems, the present invention is a cleaning method at the time of start-up of a use point pipe of a warm ultrapure water production apparatus that warms ultrapure water and supplies the ultrapure water as warm ultrapure water to the usepoint. Provided is a method for standing-up cleaning of a hot ultrapure water supply use point pipe, characterized in that the use point pipe is cleaned at a water temperature higher than the water temperature.
上記発明（請求項１）によれば、短期間で比抵抗等の水質を改善することができ、温超純水製造装置の立ち上げ期間の短縮を図ることができる。これは、以下のような理由による。すなわち、温超純水の立上洗浄時における送り温超純水と戻り温超純水における金属、カチオン、アニオン及びシリカの分析を行った結果、戻り温超純水のフッ素の濃度が非常に高く、かつ送り温超純水よりも増加していることがわかった。このことから、フッ素を原材料として含むユースポイント配管であるＰＶＤＦ配管からフッ素が溶出することによる影響であると考えられる。そうすると、このフッ素の溶出は、材料に起因するものであることから薬品等による洗浄は効果がなく、溶出が収まるまで温超純水を流通させる。このとき、通常、立上洗浄は、ユースポイントに供給する温超純水と同じ温度の超純水を流通させるが、ＰＶＤＦ配管からのフッ素の溶出は、洗浄水としての温超純水の温度が高い方が促進されることから、これよりも高い温度の水を流通することにより、フッ素の溶出を促進し、短期間でこの溶出を低減して所望の水質とすることができると考えられる。 According to the above invention (invention 1), water quality such as specific resistance can be improved in a short period of time, and the startup period of the warm ultrapure water production apparatus can be shortened. This is due to the following reasons. That is, as a result of analysis of metals, cations, anions and silica in the feed temperature ultrapure water and the return temperature ultrapure water during the on-site cleaning of the warm ultrapure water, the concentration of fluorine in the return temperature ultrapure water is very high and higher than It turns out that it is increasing. From this, it is thought that it is the influence by fluorine eluting from PVDF piping which is a use point piping containing fluorine as a raw material. Then, since the elution of fluorine is caused by the material, cleaning with chemicals or the like is not effective, and warm ultrapure water is circulated until the elution is stopped. At this time, normally, in the start-up cleaning, ultrapure water having the same temperature as the warm ultrapure water supplied to the use point is circulated. However, elution of fluorine from the PVDF pipe is performed when the temperature of the warm ultrapure water as the wash water is higher. Since it is promoted, it is considered that by flowing water at a temperature higher than this, elution of fluorine can be promoted, and this elution can be reduced in a short period of time to obtain a desired water quality.
上記発明（請求項１）においては、前記ユースポイント配管が、ＰＶＤＦからなるのが好ましい（請求項２）。 In the said invention (invention 1), it is preferable that the said use point piping consists of PVDF (invention 2).
上記発明（請求項２）によれば、ＰＶＤＦからフッ素の溶出量を短期間で低減して所望の水質とすることができ、立上期間を短縮することができる。 According to the said invention (invention 2), the elution amount of fluorine from PVDF can be reduced in a short period to obtain a desired water quality, and the start-up period can be shortened.
上記発明（請求項１，２）においては、前記立上洗浄の水温が、ユースポイントへ供給する温超純水の温度よりも５℃以上高いのが好ましい（請求項３）。具体的には、前記ユースポイントへ供給する温超純水の温度が７５℃以下であり、前記立上洗浄の水温が８０℃以上であればよい（請求項４）。 In the said invention (invention 1,2), it is preferable that the temperature of the said start-up washing is 5 degreeC or more higher than the temperature of the warm ultrapure water supplied to a use point (invention 3). Specifically, the temperature of the ultra-pure water supplied to the use point may be 75 ° C. or lower, and the temperature of the rising cleaning water may be 80 ° C. or higher.
上記発明（請求項３，４）によれば、立上洗浄の水温をユースポイントへ供給する温超純水の温度よりも５℃以上高くすることにより、フッ素の溶出を促進して短期間でフッ素溶出量を低減して所望の水質とすることができる。
According to the above inventions (
さらに、上記発明（請求項１〜４）においては、前記立上洗浄を２週間以上行うのが好ましい（請求項５）。通常、フッ素溶出量の低減には１月以上を要するが、上述したような方法を採用することにより２週間程度でフッ素の溶出量を低減することができる。 Furthermore, in the said invention (invention 1-4), it is preferable to perform the said starting washing | cleaning for 2 weeks or more (invention 5). Usually, it takes one month or more to reduce the fluorine elution amount, but by adopting the method as described above, the elution amount of fluorine can be reduced in about two weeks.
温超純水の立上洗浄時における洗浄水の水温をユースポイントに供給する温超純水よりも高温とすることで、ユースポイント配管からの不純物の溶出を促進して、短期間で低減し、これにより短期間で所望の水質とすることができる。これにより立ち上げまでの期間を短縮することができる。 The temperature of cleaning water at the time of on-site cleaning of hot ultrapure water is set to a temperature higher than that of hot ultrapure water that supplies the use point, thereby facilitating the elution of impurities from the use point piping and reducing it in a short period of time. The desired water quality can be achieved. Thereby, the period until the start-up can be shortened.
以下、本発明の温超純水供給ユースポイント配管の立上洗浄方法の実施形態について図面に基づいて詳細に説明する。 DETAILED DESCRIPTION OF THE INVENTION Embodiments of a method for rising and cleaning a hot ultrapure water supply use point pipe according to the present invention will be described in detail with reference to the drawings.
図１は、本実施形態の温超純水供給ユースポイント配管の立上洗浄方法を適用可能な、温超純水製造装置を示すフロー図である。 FIG. 1 is a flow diagram showing a hot ultrapure water production apparatus to which the hot cleaning method for hot ultrapure water supply use point piping according to this embodiment can be applied.
図１において、温超純水製造装置は、原水槽Ｔと、前処理装置１と、一次純水製造システム２と、サブシステム３とから構成されている。さらに、サブシステム３は、一次純水製造システム２の一次純水が貯留されるサブタンク４と、デミナ（非再生型イオン交換樹脂塔）５と、紫外線処理装置（ＵＶ）６と、超純水加熱装置７と、フィルタ装置（ＵＦ）８とからなる。
In FIG. 1, the warm ultrapure water production apparatus includes a raw water tank T, a pretreatment device 1, a primary pure water production system 2, and a
このようなシステム構成において、一次純水はラインＬ１を通って、サブシステム３に送られ、サブタンク４からラインＬ２を通って超純水加熱装置７に送られる。そして、超純水加熱装置７で加熱された温超純水Ｗ２がフィルタ装置（ＵＦ）８を経てユースポイント配管であるラインＬ３からユースポント９に供給され、さらに、ラインＬ４からサブタンク４に還流される。なお、１０は還流ラインＬ４に設けられた熱交換器である。
In such a system configuration, the primary pure water is sent to the
この温超純水製造装置において、超純水加熱装置７より下流側に位置するラインＬ３及びラインＬ４としては、ポリフッ化ビニリデン（ＰＶＤＦ）、テトラフルオロエチレン−パーフルオロアルキルビニルエーテル共重合体（ＰＦＡ）、テトラフルオロエチレン−ヘキサフルオロプロピレン共重合体（ＦＥＰ）等のフッ素系樹脂を内面に配した配管、特にポリフッ化ビニリデン（ＰＶＤＦ）製の配管を用いることができる。また、超純水加熱装置７より上流側のラインＬ１，Ｌ２としては、上述したフッ素系樹脂の配管の他、塩ビ配管等を用いることができる。 In this warm ultrapure water production apparatus, the lines L3 and L4 located on the downstream side of the ultrapure water heating apparatus 7 include polyvinylidene fluoride (PVDF), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), tetra A pipe having a fluorine resin such as fluoroethylene-hexafluoropropylene copolymer (FEP) arranged on the inner surface, particularly a pipe made of polyvinylidene fluoride (PVDF) can be used. Moreover, as the lines L1 and L2 on the upstream side of the ultrapure water heating device 7, a polyvinyl chloride pipe or the like can be used in addition to the above-described fluororesin pipe.
このような温超純水製造装置において、原水槽Ｔから供給された原水Ｗ０は、前処理装置１及び一次純水製造システム２で処理されて一次純水Ｗ１としてサブシステム３に供給され、サブシステム３の超純水加熱装置７で６５〜７５℃程度に加熱された後、温超純水Ｗ２としてラインＬ３からユースポント９に供給され、未使用分はラインＬ４からサブタンク４に還流される。
In such a warm ultrapure water production apparatus, the raw water W0 supplied from the raw water tank T is processed by the pretreatment apparatus 1 and the primary pure water production system 2 and supplied to the
次に上述したような温超純水製造装置のユースポイント配管の立上洗浄方法について説明する。まず、サブシシテム３に供給された一次純水Ｗ１をサブシステム３の超純水加熱装置７で加熱する。
Next, a method for cleaning up the use point piping of the above-described warm ultrapure water production apparatus will be described. First, the primary pure water W <b> 1 supplied to the
このとき、通常は、運転時の温超純水Ｗ２と同じ温度の洗浄水により立上洗浄を行うが、本実施形態においては、超純水加熱装置７で運転時にラインＬ３に供給される温超純水Ｗ２の温度よりも高い温度にまで加熱する。 At this time, normally, the on-site cleaning is performed with the cleaning water having the same temperature as the warm ultrapure water W2 at the time of operation, but in this embodiment, the warm ultrapure water W2 supplied to the line L3 at the time of operation by the ultrapure water heating device 7. Heat to a temperature higher than
これは、以下のような理由による。すなわち、ユースポイント配管であるラインＬ３はＰＶＤＦ配管であり、このラインＬ３を、加温されることによりさらに溶解性が高められた温超純水Ｗ２が流通することで、ＰＶＤＦ配管から微量のフッ素が溶出する。そこで、温超純水Ｗ２よりも高温の洗浄水で立上洗浄を行うことにより、ＰＶＤＦ配管製のラインＬ３からのフッ素の溶出が促進される結果、短期間でフッ素の溶出量を低減して、所望の水質とすることができ、これにより、立上期間の短縮を図ることができる。 This is due to the following reasons. That is, the line L3, which is a point-of-use pipe, is a PVDF pipe, and a very small amount of fluorine is eluted from the PVDF pipe by circulating warm ultrapure water W2 whose solubility is further improved by heating the line L3. To do. Therefore, by performing on-site cleaning with cleaning water having a temperature higher than that of the ultra-pure water W2, the elution of fluorine from the PVDF piping line L3 is promoted, so that the elution amount of fluorine can be reduced in a short period of time. Therefore, the start-up period can be shortened.
この場合においては、特に、温超純水Ｗ２の温度よりも５℃以上高い温度の洗浄水を供給するのが好ましい。洗浄水の温度が温超純水Ｗ２の温度よりも高ければ、ある程度の立上期間の短縮効果が得られるが、５℃未満では顕著な効果が得られないため好ましくない。具体的には、温超純水Ｗ２の温度が６５〜７５℃程度であることから、洗浄水の温度を８０℃以上に設定すればよい。 In this case, it is particularly preferable to supply cleaning water having a temperature 5 ° C. or more higher than the temperature of the warm ultrapure water W2. If the temperature of the washing water is higher than the temperature of the ultra-high purity water W2, a certain shortening effect of the start-up period can be obtained, but if it is less than 5 ° C., a remarkable effect cannot be obtained, which is not preferable. Specifically, since the temperature of the ultra-pure water W2 is about 65 to 75 ° C, the temperature of the cleaning water may be set to 80 ° C or higher.
上述したように８０℃以上の洗浄水を用いることにより、２週間以上の洗浄で温超純水製造装置の立上洗浄を完了することができ、温超純水Ｗ２と同じ温度の洗浄水を用いた場合と比べて立上期間を約半分とすることができる。 As described above, by using cleaning water at 80 ° C. or higher, it is possible to complete the start-up cleaning of the warm ultrapure water production apparatus by cleaning for two weeks or more, and using the cleaning water having the same temperature as the warm ultrapure water W2. In comparison, the startup period can be halved.
以上、本発明の実施形態について添付図面を参照して説明してきたが、本発明は前記実施形態に限定されず、種々の変更が可能である。例えば、前処理装置１、一次純水製造システム２の構成は特に制限されず、種々の構成とすることができる。また、サブシステム３についても超純水加熱装置７を備えていれば、その構成は特に制限されない。さらに、洗浄水としては、温度が相違する以外は温超純水Ｗ２と同じ水質のものを用いることができる。
As mentioned above, although embodiment of this invention has been described with reference to an accompanying drawing, this invention is not limited to the said embodiment, A various change is possible. For example, the configurations of the pretreatment device 1 and the primary pure water production system 2 are not particularly limited, and various configurations can be adopted. Further, the configuration of the
以下、実施例によって本発明を具体的に説明するが、本発明は、下記の各実施例に何ら限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited to each following Example at all.
〔実機による金属、カチオン、アニオン、シリカの分析〕
図１に示すようなシステム構成の温超純水製造装置を用いて、フィルタ装置（ＵＦ）８の出口温度約７５℃の温超純水を製造し、戻り超純水（ラインＬ４）及び送り温超純水（フィルタ装置（ＵＦ）８の出口）の各種金属、カチオン、アニオン及びシリカの濃度を測定した。
結果を表１に示す。
[Analysis of metals, cations, anions, and silica using actual equipment]
1 is used to produce warm ultrapure water having an outlet temperature of about 75 ° C. of the filter device (UF) 8 and return ultrapure water (line L4) and feed ultrapure water (filter). The concentrations of various metals, cations, anions and silica in the apparatus (UF) 8 outlet) were measured.
The results are shown in Table 1.
表１から、戻り温超純水において、Ｆの濃度が１００ｎｇ／Ｌ（ｐｐｔ）と非常に高くなっていることがわかる。しかも、送り温超純水よりもＦの濃度が増加していることから、ランイＬ３及びラインＬ４のＰＶＤＦ配管からのフッ素の溶出の影響であると推測できる。 From Table 1, it can be seen that in the return temperature ultrapure water, the concentration of F is as high as 100 ng / L (ppt). And since the density | concentration of F is increasing rather than feed temperature ultrapure water, it can be estimated that it is the influence of the elution of the fluorine from the PVDF piping of run L3 and line L4.
〔ＰＶＤＦ配管の温度の違いによる溶出特性測定試験〕
長さ１００ｃｍのＰＶＤＦ配管（内径２５ｍｍΦ、外径３１ｍｍΦ）を０．３ｍ３の２０℃及び８０℃の超純水にそれぞれ浸漬して、１日、２〜７日間、８〜３０日間のＰＶＤ配管からの各種イオン等の溶出濃度を測定するとともに溶出速度を算出した。
結果を表２に示す。
[Elution characteristics measurement test by PVDF piping temperature difference]
Length 100cm of PVDF tubing (inner diameter 25 mm, outer diameter 31Mmfai) by respectively immersing in 20 ° C. and 80 ° C. ultrapure water 0.3 m 3, 1 days, 2-7 days, PVD piping 8 to 30 days The elution concentration of various ions and the like was measured and the elution rate was calculated.
The results are shown in Table 2.
表２から、ＰＶＤＦ配管からの溶出物としてはフッ素（Ｆ）が最も多く、しかも２０℃と８０℃との間のフッ素の溶出濃度は２〜７日間で２桁、８〜３０日でも１桁高くなっており、温度による影響も大きいことがわかる。 From Table 2, fluorine (F) is the most eluent from PVDF piping, and the elution concentration of fluorine between 20 ° C and 80 ° C is 2 digits in 2-7 days, and 1 digit in 8-30 days. It is high and it can be seen that the influence of temperature is large.
〔実施例１及び比較例１〕
図１に示すようなシステム構成の温超純水製造装置において、超純水加熱装置７による温超純水の温度を８０℃として立上洗浄を７日及び１４日行った際の戻り温超純水におけるフッ素濃度及び比抵抗値を測定した（実施例１）。
結果を表３に示す。
[Example 1 and Comparative Example 1]
In the hot ultrapure water production apparatus having the system configuration shown in FIG. 1, the fluorine concentration in the return ultrapure water when the temperature of the ultrapure water by the ultrapure water heater 7 is 80 ° C. The specific resistance value was measured (Example 1).
The results are shown in Table 3.
また、比較のために通常の立上洗浄条件として、温超純水の温度を７０℃として同様に立上洗浄を７日及び１４日行った際の戻り温超純水におけるフッ素濃度及び比抵抗値を測定した（比較例１）。
結果を表３にあわせて示す。
In addition, for comparison, as a normal start-up cleaning condition, the temperature of the ultra-pure water was set to 70 ° C. and the start-up cleaning was performed on the 7th and 14th in the same manner, and the fluorine concentration and the specific resistance value in the return-temperature ultrapure water were measured. (Comparative Example 1).
The results are shown in Table 3.
表３から、８０℃で立上洗浄を行った実施例１では、戻り温超純水のフッ素濃度が１４日後には７日後と比べて大幅に低減し、比抵抗値も１８．２ＭΩ・ｃｍ以上であったのに対し、７０℃で立上洗浄を行った比較例１では、戻り温超純水のフッ素濃度の低減が十分でなく、比抵抗値は１７．８ＭΩ・ｃｍであり、１８．２ＭΩ・ｃｍ以上となるまでには５０日間必要であった。 From Table 3, in Example 1 where the start-up cleaning was performed at 80 ° C., the fluorine concentration of the return temperature ultrapure water was significantly reduced after 14 days compared to 7 days later, and the specific resistance value was 18.2 MΩ · cm or more. On the other hand, in Comparative Example 1 in which the startup cleaning was performed at 70 ° C., the fluorine concentration of the return temperature ultrapure water was not sufficiently reduced, and the specific resistance value was 17.8 MΩ · cm, and 18.2 MΩ · cm. It took 50 days to reach this point.
７…超純水加熱装置
９…ユースポイント
Ｌ３…ライン（ユースポイント配管）
Ｗ２…温超純水
7 ... Ultrapure water heating device 9 ... Use point L3 ... Line (use point piping)
W2 ... Warm ultrapure water
Claims (5)
供給する温超純水の水温よりも高い水温で前記ユースポイント配管の洗浄を行うことを特徴とする温超純水供給ユースポイント配管の立上洗浄方法。 A cleaning method at the time of start-up of a use point pipe of a warm ultra pure water production apparatus that heats ultra pure water and supplies it to the use point as warm ultra pure water,
A method for standing and cleaning a hot ultrapure water supply use point pipe, wherein the use point pipe is cleaned at a temperature higher than the temperature of the supplied hot ultra pure water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008298635A JP5527502B2 (en) | 2008-11-21 | 2008-11-21 | Hot ultrapure water supply use point piping startup cleaning method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008298635A JP5527502B2 (en) | 2008-11-21 | 2008-11-21 | Hot ultrapure water supply use point piping startup cleaning method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2010123897A true JP2010123897A (en) | 2010-06-03 |
| JP5527502B2 JP5527502B2 (en) | 2014-06-18 |
Family
ID=42324948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2008298635A Active JP5527502B2 (en) | 2008-11-21 | 2008-11-21 | Hot ultrapure water supply use point piping startup cleaning method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP5527502B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018020272A (en) * | 2016-08-02 | 2018-02-08 | オルガノ株式会社 | Ultrapure water production device and ultrapure water production method |
| KR20210149654A (en) * | 2020-06-02 | 2021-12-09 | 주식회사 케이씨 | Apparatus and Method for cleaning a coupler of chemical supply device |
| JP7033691B1 (en) | 2021-10-29 | 2022-03-10 | 野村マイクロ・サイエンス株式会社 | How to start up the warm ultra-pure water production system, start-up program, and warm ultra-pure water production system |
| KR20240049192A (en) | 2022-10-07 | 2024-04-16 | 노무라마이크로사이엔스가부시키가이샤 | Sterilization method for pharmaceutical water production system and pharmaceutical water production system |
| KR20240049189A (en) | 2022-10-07 | 2024-04-16 | 노무라마이크로사이엔스가부시키가이샤 | Sterilization method for pharmaceutical water production system |
| KR20240049186A (en) | 2022-10-07 | 2024-04-16 | 노무라마이크로사이엔스가부시키가이샤 | Pharmaceutical water production system and Method of operating pharmaceutical water production system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07195073A (en) * | 1994-01-06 | 1995-08-01 | Japan Organo Co Ltd | Method for washing ultra-pure water producing apparatus |
| JP2000317413A (en) * | 1999-05-14 | 2000-11-21 | Kurita Water Ind Ltd | Method for washing ultrapure water production system |
-
2008
- 2008-11-21 JP JP2008298635A patent/JP5527502B2/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07195073A (en) * | 1994-01-06 | 1995-08-01 | Japan Organo Co Ltd | Method for washing ultra-pure water producing apparatus |
| JP2000317413A (en) * | 1999-05-14 | 2000-11-21 | Kurita Water Ind Ltd | Method for washing ultrapure water production system |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018020272A (en) * | 2016-08-02 | 2018-02-08 | オルガノ株式会社 | Ultrapure water production device and ultrapure water production method |
| KR20210149654A (en) * | 2020-06-02 | 2021-12-09 | 주식회사 케이씨 | Apparatus and Method for cleaning a coupler of chemical supply device |
| KR102412782B1 (en) * | 2020-06-02 | 2022-06-27 | 주식회사 케이씨 | Apparatus and Method for cleaning a coupler of chemical supply device |
| JP7033691B1 (en) | 2021-10-29 | 2022-03-10 | 野村マイクロ・サイエンス株式会社 | How to start up the warm ultra-pure water production system, start-up program, and warm ultra-pure water production system |
| JP2023066522A (en) * | 2021-10-29 | 2023-05-16 | 野村マイクロ・サイエンス株式会社 | Hot ultrapure water production system startup method, startup program, and hot ultrapure water production system |
| US11926536B2 (en) | 2021-10-29 | 2024-03-12 | Nomura Micro Science Co., Ltd. | Method for starting up hot ultrapure water production system, and hot ultrapure water production system |
| KR20240049192A (en) | 2022-10-07 | 2024-04-16 | 노무라마이크로사이엔스가부시키가이샤 | Sterilization method for pharmaceutical water production system and pharmaceutical water production system |
| KR20240049189A (en) | 2022-10-07 | 2024-04-16 | 노무라마이크로사이엔스가부시키가이샤 | Sterilization method for pharmaceutical water production system |
| KR20240049186A (en) | 2022-10-07 | 2024-04-16 | 노무라마이크로사이엔스가부시키가이샤 | Pharmaceutical water production system and Method of operating pharmaceutical water production system |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5527502B2 (en) | 2014-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5527502B2 (en) | Hot ultrapure water supply use point piping startup cleaning method | |
| TW418357B (en) | Chemical generator with controlled mixing and concentration feedback and adjustment | |
| JP4480061B2 (en) | Ultrapure water production apparatus and cleaning method for ultrapure water production and supply system in the apparatus | |
| TWI801568B (en) | Manufacturing method of heated ozone water, heated ozone water and semiconductor wafer cleaning solution | |
| TW201501195A (en) | Processing system and method for providing a heated etching solution | |
| TW201520175A (en) | Ultrapure water production system, ultrapure water production supply system, and method for cleaning same | |
| JP2009260020A (en) | Cleaning water for electronic material, method of cleaning electronic material, and system for supplying water containing dissolved gas | |
| JP2006066727A (en) | Semiconductor manufacturing device and chemical exchanging method | |
| TW201902562A (en) | Cleaning method of hollow fiber membrane device, ultrafiltration membrane device, ultrapure water manufacturing device and hollow fiber membrane device cleaning device | |
| TW201836993A (en) | DILUTED CHEMICAL LIQUID PRODUCTION APPARATUS CAPABLE OF CONTROLLING pH AND OXIDATION-REDUCTION POTENTIAL | |
| JP6427378B2 (en) | Ammonia dissolved water supply system, ammonia dissolved water supply method, and ion exchange apparatus | |
| JP2011161418A (en) | Washing method for ultrapure water production system | |
| JP2009189905A (en) | Heat recovery type cleaning equipment | |
| JP2000290693A (en) | Cleaning of electronic parts and members | |
| JP2010135810A (en) | METHOD OF CONTROLLING pH VALUE OF SOLUTION AND OXIDATION-REDUCTION POTENTIAL, AND APPARATUS | |
| JP6107987B1 (en) | Cleaning method of ultrapure water production system | |
| JP2000317413A (en) | Method for washing ultrapure water production system | |
| JP6206173B2 (en) | Semiconductor wafer cleaning method | |
| JP6149421B2 (en) | Solution supply method and supply device | |
| US9875915B2 (en) | Method for removing metal contamination and apparatus for removing metal contamination | |
| JP7480594B2 (en) | Electronic component cleaning water manufacturing equipment | |
| TWI793049B (en) | Method for starting up hot ultrapure water production system, starting up program, and hot ultrapure water production system | |
| JP7099603B1 (en) | Liquid supply equipment for semiconductor manufacturing | |
| JP2022187148A (en) | Method for starting up water treatment device and washing method | |
| JP2007260211A (en) | Method for antiseptically cleaning ultrapure water producing system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20111018 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20121225 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20130109 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20130308 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20130911 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20140319 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20140401 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 5527502 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |