TW201836994A - 規定濃度水的供給方法及裝置 - Google Patents
規定濃度水的供給方法及裝置 Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 131
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 31
- 239000012498 ultrapure water Substances 0.000 claims abstract description 31
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- 238000003860 storage Methods 0.000 claims description 29
- 238000001514 detection method Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
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- 238000002835 absorbance Methods 0.000 description 1
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- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 description 1
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Abstract
一種規定濃度水的供給方法及裝置,具有對超純水添加導電性的第1液、與非導電性的第2液之至少2種類的液來製造含有規定濃度的第1液成分及第2液成分之規定濃度水之工程,該規定濃度水的供給方法,係事先調製將該第1液與第2液預先以規定混合比混合而成之混合液,將該混合液添加至超純水,使得添加後的超純水的導電率或電阻率成為規定值。
Description
[0001] 本發明係用來供給規定濃度的水之方法及裝置,特別有關將導電性的第1液、與非導電性的第2液混合而添加至超純水來調製、供給規定濃度的水之規定濃度水的供給方法及裝置。 [0002] 更詳言之,本發明有關適合供給半導體用晶圓的洗淨/淋洗(rinse)工程中有效之,含有鹼/氧化劑等極低濃度的溶質之洗淨水的方法及裝置。
[0003] 半導體用矽晶圓等的洗淨及淋洗工程中,有時會使用將有助於pH或氧化還原電位的控制之溶質予以溶解極低濃度而成的水(在此稱為稀薄洗淨水)。以超純水作為基本材料,為了使其帶有符合洗淨或淋洗等工程之目的的pH或氧化還原電位等液特性,會添加必要最小限度的酸/鹼、氧化劑/還原劑。有令H2
、NH3
、O3
這些還原性、鹼性、酸性的氣體溶解於超純水之方法,但微量添加藥液(注藥)之方法亦簡便,受到活用。 [0004] 作為注藥之方法,有使用泵浦之方法、使用密閉容器與N2
等惰性氣體所造成的加壓之方法,已各自實用化。 [0005] 稀薄洗淨水之供給中,為使溶質濃度落在期望範圍,會依各式各樣的手法做溶解控制,如接收濃度監控器的訊號之PID控制、對於超純水流量之比例控制等。就半導體的洗淨工程中常被使用的藥液的一種而言可舉出H2
O2
,即使在洗淨機中使用的流量有變動的情形下仍經常要求嚴格的濃度控制。惟不會以H2
O2
單獨用於洗淨,而是常和酸、鹼等藥液混合使用。 [0006] 作為測定H2
O2
的濃度之方法,使用比色滴定之方法為主流,作為線上(online)監控之方法,有由平沼產業(股)販賣之「Process Titrator AHP310」。此外有由Aero Laser GmbH販賣之同樣運用了吸光光度的「AL2021」。但該些方法中,為了測定必須使用規定的試藥,試藥管理及調整會變得繁雜。 [0007] 日本特開2012-63303號公報中,記載著令水中的過氧化氫分解,測定溶氧的濃度,藉此無須使用試藥而將H2
O2
濃度定量,但需要脫氣裝置而裝置會變得繁雜、及會依賴DO計的靈敏度,因此有無法正確地計測低濃度域之問題。 [0008] 像這樣,習知的方法中,當洗淨機中使用的流量有變動的情形下,無法經常做嚴格的濃度控制。此外,不能充分進行ppb位準下的PID控制,無法做微量濃度域的控制。其結果,澆注於晶圓之洗淨水/淋洗水的液質,一直停留在和理想值相距甚遠之廣範圍下的控制。 [0009] 雖然也有以液質穩定化為優先,事先以一定的條件製造稀薄洗淨水,貯藏之,而從貯藏槽持續供給的單純方法,但在此情形下,必須將大規模的貯水槽設置於製造晶圓之無塵室內的洗淨機附近,而不切實際。 [0010] 專利文獻1:日本特開2012-63303號公報
[0011] 本發明,目的在於提供一種將導電性的第1液、與非導電性的第2液混合以規定濃度添加至超純水而有效率地製造、供給規定濃度水之規定濃度水的供給方法及裝置。本發明,於其一個態樣中,目的在於提供一種有效率地製造、供給以規定濃度含有H2
O2
的稀薄洗淨水之規定濃度水的供給方法及裝置。 [0012] 本發明之規定濃度水的供給方法,具有對超純水添加導電性的第1液、與非導電性的第2液之至少2種類的液來製造含有規定濃度的第1液成分及第2液成分之規定濃度水之工程,該規定濃度水的供給方法,其特徵為,事先調製將該第1液與第2液預先以規定混合比混合而成之混合液,將該混合液添加至超純水,使得添加後的超純水的導電率或電阻率成為規定值。 [0013] 本發明之規定濃度水的供給裝置,係具備下述而成:導電性的第1液與非導電性的第2液之至少2種類的液以規定混合比混合而成之混合液的貯留槽;及用來將該貯留槽內的混合液注藥至超純水之混合液送液手段;及計測被注藥了混合液的超純水的導電率或電阻率之導電率計或電阻率計;及計測被注藥了混合液的超純水的瞬間流量之瞬間流量計;及控制前述混合液送液手段以使該導電率計或電阻率計的檢測值成為規定之控制手段。 [0014] 本發明的一個態樣中,第1液為酸或鹼的水溶液,第2液為H2
、H2
O2
或O3
的溶解水。發明之功效
[0015] 按照本發明,是將把導電性的第1液、與非導電性的第2液預先以規定混合比混合而成之混合液添加至超純水,使得添加後的該超純水的導電率或電阻率成為規定值,故能夠有效率地製造第1液及第2液各自以規定濃度添加至超純水而成之規定濃度水。 [0016] 稀薄洗淨水的溶解成分中,有NH3
等的鹼,HCl、H2
SO4
、HF等的酸、H2
O2
等的氧化劑這些藉由一般性的EL級(電子工業級)的藥液添加而供給之物,或O3
、H2
、CO2
這些藉由氣體溶解而供給之物。它們任一者均頂多是ppm~ppb尺度下的添加,藉此修正液質。當線上監控ppm尺度下的添加的情形下,導電率計因其響應性佳、且構造簡便無耗材而合適,但H2
O2
難以被導電率計檢測。另一方面,NH3
或HCl、CO2
等若為ppm尺度則可藉由導電率計高靈敏度地檢測。此外,當監控ppb尺度下的添加的情形下,可使用電阻率計來代替導電率計。此電阻率計響應性佳,且構造簡便無耗材因此合適。 [0017] 按照本發明,是將能夠藉由導電率計監控添加量之導電性的第1液、與難以藉由導電率計監控之非導電性的第2液於事前以規定比率事先混合,於混合液注藥後藉由導電率計或電阻率計監控來控制混合液的添加量,藉此能夠有效率地製造以高精度而以規定濃度含有第1液及第2液中的各成分而成之規定濃度水。
[0019] 以下參照圖面1~3說明實施形態。 [0020] 圖1中,導電性的第1液透過配管1、3被導入貯留槽6,非導電性的第2液透過配管2、3被導入貯留槽6。 [0021] 第1液及第2液對貯留槽6之供給量,是藉由累積流量計4、5各自受檢測,在貯留槽6貯留有第1液與第2液以規定的比率混合而成之混合液M。在貯留槽6設有水位感測器7。 [0022] 此貯留槽6內的混合液M,透過泵浦8及配管9,對流通於配管10之超純水在注藥點10a注藥(添加)。注藥後的超純水,藉由導電率計11被計測導電率,並且藉由瞬間流量計12被計測流量。 [0023] 導電率計11及瞬間流量計12的檢測值,被輸入至泵浦控制裝置(圖示略),泵浦控制裝置,控制泵浦8以使得導電率計11的檢測值成為規定值。 [0024] 混合液M,為第1液與第2液以規定比率混合而成之物,此混合液中的成分當中會影響導電率計11的檢測值者實質上僅有第1液。因此,若以導電率計11的檢測值成為規定值之方式進行混合液M之注藥,則注藥後的超純水中的第1液成分會成為規定濃度。此外,混合液M中的第1液與第2液之比率,是預先呈規定比率(訂為目標之規定濃度水中的第1液成分與第2液成分之比率),故注藥後的超純水中的第2液成分濃度亦會成為規定濃度。依此方式,製造恰好含有規定濃度之第1液成分及第2液成分的規定濃度水,此規定濃度水被送水至半導體製造工程的洗淨機等。 [0025] 導電率計11及瞬間流量計12的精度及響應性極高,故規定濃度水中的各成分濃度的距目標值之誤差極小。 [0026] 作為上述的第1液,可示例出氨、四烷基氫氧化銨(tetra alkyl ammonium hydroxide)、胺等的鹼性水溶液,HCl、H2
SO4
、HF、CO2
等的酸性水溶液等。作為第2液,可示例出H2
O2
、H2
、O3
等的氣體溶解水等。第1液的導電率通常為0.05~5mS/m左右。第2液的導電率通常為0.02mS/m以下。但,第2液的導電率訂為第1液的1/5以下。添加了混合液M的超純水中的第1液成分濃度即使為ppm尺度,其濃度仍會藉由導電率計而高精度地受計測。 [0027] 圖1中,是藉由使用累積流量計4、5,來將貯留槽6內的混合液M中的第1液與第2液之混合比做成規定比,但圖2中,是構成為在貯留槽6設置重量感測器20,對該貯留槽6導入了規定量a的第1液之後(或之前),對貯留槽6導入規定量b的第2液,藉此令第1液與第2液之混合比a/b呈規定值的混合液M貯留於貯留槽6。其他的構成和圖1相同。 [0028] 圖1、2中是藉由泵浦8進行注藥,但亦可設計成如圖3般將惰性氣體(例如氮、氦等)供給至貯留槽6,藉由惰性氣體壓將貯留槽6內的混合液M注藥至超純水,而省略泵浦8。圖3的其他的構成和圖1相同。圖3是設計成在圖1的系統中利用惰性氣體壓之構成,但圖2的系統亦能同樣地構成。 [0029] 本發明中,能夠直接利用習知的注藥機構。亦即,本發明裝置,是具備用來將相異2種類的藥液的比率經常設為規定的值之累積流量計4、5、及用來監視混合液的水位之水位感測器7、及用來貯留混合液之貯留槽6、及用來從貯留槽6送液至注藥點10a之送液泵浦8或惰性氣體壓送手段、及用來監控和超純水混合後的導電率之導電率計11、及用來監視送水量之瞬間流量感測器12等,而該些機器依靠習知的注藥機構之物即足夠。另,在規定濃度水的送水管線的途中亦可設置用來除去雜質之過濾器等單元。 [0030] 藉由將累積流量計4、5與水位感測器7組合,能夠對貯留槽6自動地供給2種類的藥液。混合液M,不限定於2種類的液的混合液,亦可為3種類以上的複數藥液的混合液。 [0031] 藉由將送液泵浦8與導電率計11與瞬間流量感測器12組合,而做PID控制或比例控制,即使當流量有變動的情形下仍可經常做嚴格的濃度控制。不會因藥液的黏度、比重而損及控制性。另,以上雖針對使用了導電率計11之情形來說明,但當為ppb尺度的情形下,只要使用電阻率計來代替導電率計11即可。實施例
[0032] [實施例1] 圖1的系統中,以下述條件對超純水進行了注藥。結果如表1所示。 [0033] 超純水送水量:12~20L/min 第1液:NH4
OH 10ppm水溶液 第2液:H2
O2
1ppm溶解水 泵浦8的控制方式:PID 試驗時間:20分鐘 [0034] [實施例2] 如圖2般使用了重量感測器20來代替累積流量計4、5,除此以外以和實施例1相同條件進行了注藥。結果如表1所示。 [0035] [實施例3] 省略泵浦8,使用了圖3的惰性氣體壓送方式之系統,除此以外以和實施例1相同條件進行了注藥。結果如表1所示。 [0036] [實施例4] 實施例3中,如圖2般使用了重量感測器20來代替累積流量計4、5,除此以外以同一條件進行了注藥。結果如表1所示。 [0037] [比較例1] 如圖4所示,使用了設計成下述般之系統,即,對貯留槽6僅供給第1液,而對另行設置之第2貯留槽6A僅供給第2液,將第1液透過泵浦8在注藥點10a注藥,針對第2液則透過第2泵浦8A在第2注藥點10b注藥。非導電性之第2液的濃度計測是使用線上H2
O2
監控器13進行。此時的瞬間流量是使用瞬間流量計14計測。其他則以和實施例1相同條件進行了注藥。結果如表1所示。 [0038][0039] 如表1般,實施例1~4和併設第2貯留槽6、6A之習知方式具有同等的注藥性能。 [0040] 由以上的實施例1~4、比較例1即可明白,藉由將以導電率計計測出的值用於PID控制,能夠實現將計測困難的非導電性的H2
O2
、及導電性的藥液精度良好而穩定地供給,而將洗淨/淋洗工程中極為重要的液質設為期望之值。此外當比例控制的情形下,藉由反映導電率計的測定結果來調節注藥量,亦能穩定地供給。 [0041] [實驗例1] 針對貯留槽中下記的濃厚藥液(混合液)中的各成分的自我分解性,依以下條件計測。結果如圖5所示。 [0042] 槽容量:10L NH4
OH濃度:25wt% H2
O2
濃度:30wt% 外氣溫:25℃ 保管期間:1個月 檢測方法:比色滴定 如圖5般,可知即使在混合了濃厚藥液的狀態下,5日內仍濃度一定。由此,可知槽貯留量設計成為5日以下,藉此便不必對每種藥液設置槽及注藥點。此外當槽貯留量變得低於規定之值的情形下,判斷能夠藉由使用累積式流量計或重量計補充各藥液而解決。 [0043] 雖已利用特定的態樣詳細說明了本發明,但所屬技術領域者當知可不脫離本發明之意圖與範圍而做各式各樣的變更。 本申請案,奠基於2017年3月30日申請之日本特許申請案2017-068091,其全體藉由引用而被援用。
[0044]
4、5‧‧‧累積流量計
6、6A‧‧‧貯留槽
11‧‧‧導電率計
13‧‧‧H2O2監控器
12、14‧‧‧瞬間流量計
[0018] [圖1] 第1實施形態之規定濃度水的供給方法及裝置的說明圖。 [圖2] 第2實施形態之規定濃度水的供給方法及裝置的說明圖。 [圖3] 第3實施形態之規定濃度水的供給方法及裝置的說明圖。 [圖4] 比較例的說明圖。 [圖5] 實驗結果示意圖表。
Claims (4)
- 一種規定濃度水的供給方法,具有對超純水添加導電性的第1液、與非導電性的第2液之至少2種類的液來製造含有規定濃度的第1液成分及第2液成分之規定濃度水之工程,該規定濃度水的供給方法,其特徵為, 事先調製將該第1液與第2液預先以規定混合比混合而成之混合液, 將該混合液添加至超純水,使得添加後的超純水的導電率或電阻率成為規定值。
- 如申請專利範圍第1項所述之規定濃度水的供給方法,其中,前述第1液為酸或鹼的水溶液,第2液為H2 、H2 O2 或O3 的溶解水。
- 一種規定濃度水的供給裝置,係具備下述而成: 導電性的第1液與非導電性的第2液之至少2種類的液以規定混合比混合而成之混合液的貯留槽;及 用來將該貯留槽內的混合液注藥至超純水之混合液送液手段;及 計測被注藥了混合液的超純水的導電率或電阻率之導電率計或電阻率計;及 計測被注藥了混合液的超純水的瞬間流量之瞬間流量計;及 控制前述混合液送液手段以使該導電率計或電阻率計的檢測值成為規定之控制手段。
- 如申請專利範圍第3項所述之規定濃度水的供給裝置,其中,前述第1液為酸或鹼的水溶液,第2液為H2 、H2 O2 或O3 的溶解水。
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