JPH06167449A - Method and equipment for controlling concentration - Google Patents
Method and equipment for controlling concentrationInfo
- Publication number
- JPH06167449A JPH06167449A JP32028292A JP32028292A JPH06167449A JP H06167449 A JPH06167449 A JP H06167449A JP 32028292 A JP32028292 A JP 32028292A JP 32028292 A JP32028292 A JP 32028292A JP H06167449 A JPH06167449 A JP H06167449A
- Authority
- JP
- Japan
- Prior art keywords
- light
- concentration
- measuring
- absorbance
- transmittance
- 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
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
- Weting (AREA)
- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
【０００１】本発明は半導体集積回路装置、液晶表示装
置の作成に際して使用する現像、エッチング、剥離、洗
浄工程において、薬液を回収、循環し要する場合の液晶
濃度管理方法および装置に関する。The present invention relates to a liquid crystal concentration control method and device for recovering and circulating a chemical solution in the developing, etching, peeling and cleaning steps used for manufacturing a semiconductor integrated circuit device and a liquid crystal display device.
【０００２】半導体集積回路装置、液晶表示装置の作成
に際して、現像、エッチング、剥離、洗浄工程が行われ
る。この場合、薬液を回収してフィルタリングし、再度
生産ラインに戻す処理がともなう。薬液は循環使用して
いるうちに被溶解物が溶け込んで活性度が低下する。そ
こで、オペレータがその薬液をサンプリングして吸光光
度分析、比色分析、比抵抗分析をおこなって薬液の寿命
をチェックして、薬液を新しいものに交換している。し
かし、この方法ではオペレータが生産ラインから薬液を
サンプリングしなければ薬液濃度のチェックができな
い。また、分析装置の校正も必要である。さらに連続的
な監視ができないので、測定の間に薬液が劣化し、新液
交換が遅くなってしまう場合もあった。Development of a semiconductor integrated circuit device and a liquid crystal display device involves development, etching, peeling and cleaning steps. In this case, the process involves collecting the chemical solution, filtering it, and returning it to the production line again. The activity of the chemical solution decreases as the substance to be dissolved dissolves in it while it is being circulated. Therefore, the operator samples the drug solution and performs absorptiometry, colorimetric analysis, and resistivity analysis to check the life of the drug solution and replace it with a new one. However, in this method, the operator cannot check the chemical concentration unless the operator samples the chemical from the production line. It is also necessary to calibrate the analyzer. Furthermore, since continuous monitoring cannot be performed, the chemical solution may deteriorate during the measurement and the replacement of the new solution may be delayed.
【０００３】本発明者らは上記の問題を解決するために
は、溶液の吸光度または透過率を測定することにより濃
度を測定することが最もよいことを見いだして本発明を
完成した。すなわち本発明は、循環利用される薬液の薬
液槽の濃度管理方法であって、溶液の吸光度または透過
率を測定して濃度を検知し管理することを特徴とする濃
度管理方法を提供するものである。さらに本発明は、上
記の方法を実施するための装置として、光源、光源に接
続された光ファイバーと末端にピックアップレンズを有
する光照射部、受光ピックアップレンズと光ファイバー
とからなる受光部、光源からの光強度および受光部で検
出された光強度を測定する光センサー、並びに前記光強
度から吸光度または透過率を得るためのコンピューター
を有する薬液の濃度測定装置を提供するものである。The present inventors have completed the present invention by finding that the best way to solve the above problems is to measure the concentration by measuring the absorbance or transmittance of a solution. That is, the present invention provides a method for controlling the concentration of a chemical solution tank for circulating and utilizing a chemical solution, which is characterized by measuring the absorbance or transmittance of the solution and detecting and controlling the concentration. is there. Furthermore, the present invention provides, as an apparatus for carrying out the above method, a light source, an optical fiber connected to the light source and a light irradiation section having a pickup lens at the end, a light receiving section composed of a light receiving pickup lens and an optical fiber, and light from the light source. Provided is an optical sensor for measuring the intensity and the light intensity detected by a light receiving section, and a concentration measuring device for a chemical solution having a computer for obtaining the absorbance or the transmittance from the light intensity.
【０００４】濃度測定に際し、本発明のように吸光度ま
たは透過率を測定せず、たとえば比抵抗測定や中和滴定
により測定することも考えられる。しかし、比抵抗を測
定する場合には測定値のバラツキが大きく、抵抗計の校
正を厳密に行う必要があり、この方法は濃度管理の手段
としては適当でない。また中和滴定による場合には、測
定毎にサンプリングをしなければならず、自動化をする
ことができないという問題点が生ずるので、本発明にお
いては吸光度または透過率を測定することとしたもので
ある。It is also conceivable to measure the concentration by measuring the specific resistance or neutralization titration without measuring the absorbance or the transmittance as in the present invention. However, when measuring the specific resistance, there is a large variation in the measured value, and it is necessary to strictly calibrate the resistance meter, and this method is not suitable as a means for controlling the concentration. Further, in the case of neutralization titration, sampling is required for each measurement, which causes a problem that automation cannot be performed. Therefore, in the present invention, the absorbance or the transmittance is measured. .
【０００５】本発明を実施するための装置の構成例を図
１に示す。装置は光源、光源に接続された光ファイバー
と末端にピックアップレンズを有する光照射部、受光ピ
ックアップレンズと光ファイバーとからなる受光部、光
源からの光強度および受光部で検出された光強度を測定
する光センサー、並びに前記光強度から吸光度または透
過率を得るためのコンピューターを含む。光源は紫外線
領域を発光するＤ２ランプまたは可視光領域を発光する
ハロゲンランプの両者が使用できる。光源は後述される
ように、必要により切り替えることができる。光源から
発せられた光は光ファイバーに入る。光ファイバーの末
端にはピックアップレンズが設けられる。光ファイバー
末端は濃度を測定する薬液に浸漬されており、ピックア
ップレンズは耐薬品性の膜により被覆されることが好ま
しい。また、光ファイバーの材質は耐食性の点から石英
光ファイバーが好ましい。また、複数の光ファイバーを
束にして使用することができる。ピックアップレンズか
ら照射された光を受光できる位置に受光部が配置され
る。受光部も、光ファイバーと末端に設けられたピック
アップレンズからなる。照射された光は光ファイバーを
出た後、薬液中を通過し、受光部を通り、光センサーで
強度が測定される。光強度はアナログデジタルコンバー
ター（以下「ＡＤＣ」）でデジタル信号に変換され、コ
ンピューターで分析される。コンピューターは通常のパ
ーソナルコンピューター（以下「ＰＣ」）が使用でき
る。光源から発せられた入射光強度を測定するために、
光源から入射光強度測定ラインが設けられ、同様に光セ
ンサーで強度を測定し、ＡＤＣを経てＰＣへデータが送
られる。入射光強度を同時に測定するので、入射光強度
の変動やランプの劣化にともなう強度変化による影響を
避けることができる。An example of the configuration of an apparatus for carrying out the present invention is shown in FIG. The device is a light source, a light emitting section having an optical fiber connected to the light source and a pickup lens at the end, a light receiving section composed of a light receiving pickup lens and an optical fiber, light intensity from the light source and light measuring the light intensity detected by the light receiving section. It includes a sensor and a computer for obtaining the absorbance or the transmittance from the light intensity. As the light source, both a D2 lamp that emits in the ultraviolet region and a halogen lamp that emits in the visible region can be used. The light source can be switched as needed, as described later. The light emitted from the light source enters the optical fiber. A pickup lens is provided at the end of the optical fiber. The end of the optical fiber is immersed in a chemical solution for measuring the concentration, and the pickup lens is preferably covered with a chemical resistant film. Further, the material of the optical fiber is preferably quartz optical fiber from the viewpoint of corrosion resistance. Also, a plurality of optical fibers can be used in a bundle. The light receiving unit is arranged at a position where the light emitted from the pickup lens can be received. The light receiving section also includes an optical fiber and a pickup lens provided at the end. The emitted light exits the optical fiber, passes through the liquid medicine, passes through the light receiving portion, and the intensity is measured by the optical sensor. The light intensity is converted into a digital signal by an analog-digital converter (hereinafter “ADC”) and analyzed by a computer. As the computer, an ordinary personal computer (hereinafter “PC”) can be used. In order to measure the intensity of the incident light emitted from the light source,
An incident light intensity measurement line is provided from the light source, the intensity is similarly measured by the optical sensor, and the data is sent to the PC via the ADC. Since the incident light intensity is measured at the same time, it is possible to avoid the influence of the variation of the incident light intensity and the intensity change due to the deterioration of the lamp.
【０００６】薬液中に照射された光は薬液中の成分によ
って光吸収される。この時、以下のようなランバートベ
ールの法則が成り立つ。The light radiated into the chemical liquid is absorbed by the components in the chemical liquid. At this time, the following Lambert Beer's law holds.
【０００７】ｌｏｇ（Ｉ0／Ｉ）＝ａｂｃ Ｔ＝１０-abc Ｉo：入射光強度 Ｉ ：透過光強度 α ：吸光係数 ｂ ：照射部と受光部の間の距離 ｃ ：濃度 Ｔ ：透過率 上記の関係を利用すれば、あらかじめｃとＴの関係を求
めた後、吸光度、すなわちｌｏｇ（Ｉ0／Ｉ）または透
過率を測定すれば、薬液中の薬品の濃度を知ることがで
きる。Log (I 0 / I) = abc T = 10 −abc I o : incident light intensity I: transmitted light intensity α: extinction coefficient b: distance between irradiation part and light receiving part c: concentration T: transmittance Using the above relationship, the concentration of the drug in the drug solution can be known by first determining the relationship between c and T and then measuring the absorbance, that is, log (I 0 / I) or transmittance.
【０００８】薬品の濃度が大きい場合には測定器の感度
がオーバーフローしてしまうことがある。通常の測定の
場合にはサンプルを希釈して濃度を感度内に落とすこと
により対処できるが、本発明にかかる装置の場合には測
定部分、すなわち光照射部および受光部がライン中の薬
液槽中に浸漬された状態で使用されるので、薬液を希釈
することができない。そこで、本発明にかかる方法にお
いては以下の２つの方法によりこの問題を解決した。そ
の２つの方法とは、１）光照射部と受光部との距離を調
節する方法、または２）測定波長を変更する方法であ
る。When the concentration of the chemical is high, the sensitivity of the measuring device may overflow. In the case of normal measurement, it can be dealt with by diluting the sample to reduce the concentration to within the sensitivity, but in the case of the device according to the present invention, the measurement part, that is, the light irradiation part and the light receiving part is in the chemical tank in the line The chemical solution cannot be diluted because it is used while being immersed in. Therefore, in the method according to the present invention, this problem is solved by the following two methods. The two methods are 1) a method of adjusting the distance between the light irradiation section and the light receiving section, or 2) a method of changing the measurement wavelength.
【０００９】上記の方法のいずれかにより、測定感度を
変更し、適正な測定をすることができる。By any of the above methods, the measurement sensitivity can be changed and proper measurement can be performed.
【００１０】さらに、薬液濃度の範囲により吸光度また
は透過率のいずれを測定するかを選択できる。一般に濃
度が一定以上になると吸光度は飽和してしまうので、そ
れ以上の濃度の場合には透過率を測定した方が好まし
い。また、一般には低濃度では紫外線領域の波長を、高
濃度では可視光領域の波長を使用した方が好ましい結果
が得られる。さらに、測定ギャップを短くすることによ
っても測定感度を変更することができる。Further, it is possible to select whether to measure the absorbance or the transmittance depending on the range of the concentration of the chemical solution. Generally, if the concentration becomes higher than a certain level, the absorbance will be saturated, so it is preferable to measure the transmittance when the concentration is higher than that. In general, it is preferable to use a wavelength in the ultraviolet range at low concentrations and a wavelength in the visible range at high concentrations. Furthermore, the measurement sensitivity can be changed by shortening the measurement gap.
【００１１】本発明にかかる方法および装置により、薬
液槽中の薬液の濃度を連続的に測定することが可能とな
った。これにより、薬液の劣化に対して迅速な対応がで
きるとともに、濃度の正確なコントロールにより工程の
安定化を図ることができる。The method and apparatus according to the present invention make it possible to continuously measure the concentration of the chemical liquid in the chemical liquid tank. As a result, it is possible to promptly deal with the deterioration of the chemical liquid and to stabilize the process by accurately controlling the concentration.
【００１２】以下に実施例に基づき本発明をより詳細に
説明する。The present invention will be described in more detail based on the following examples.
【００１３】実施例１ ノボラック系ポジ型レジスト（ｇ線レジストＯＦＰＲ−
８００（東京応化社製））を現像液（ＴＭＡＨ２．３８
％）に溶解し、以下の各条件で測定を行った。Example 1 A novolak positive resist (g-line resist OFPR-
800 (manufactured by Tokyo Ohka Co., Ltd.) as a developer (TMAH 2.38)
%) And measured under the following conditions.
【００１４】ａ）５３０，１７７０，および３５３０ｍ
ｇ／リットルの濃度で溶解した溶液について吸光度を測
定した。その結果を図２に示す。A) 530, 1770, and 3530 m
The absorbance was measured for the solution dissolved at a concentration of g / liter. The result is shown in FIG.
【００１５】ｂ）透過率を測定した場合の結果を図３に
示す。B) The results of measuring the transmittance are shown in FIG.
【００１６】低濃度では紫外線領域での吸光度を、高濃
度では可視光領域での吸光度を測定することによりすべ
ての濃度を測定することができた。このように測定波長
を変更することにより幅広い範囲の濃度を測定できるこ
とがわかる。It was possible to measure all the concentrations by measuring the absorbance in the ultraviolet region at low concentrations and the absorbance in the visible region at high concentrations. It can be seen that the concentration in a wide range can be measured by changing the measurement wavelength in this way.
【００１７】上記の実験結果を、レジスト濃度と吸光度
との関係（図４）、および透過率との関係（図５）につ
いてプロットした。どちらも濃度と直線関係にあること
が分かる。なお、濃度が２０００ｍｇ／リットル以上に
なると吸光度は飽和して変化しなくなる。したがって、
低濃度領域では吸光度を測定するのがよく、高濃度領域
では透過率を測定するのがよいとわかる。The above experimental results were plotted with respect to the relationship between the resist concentration and the absorbance (FIG. 4) and the relationship with the transmittance (FIG. 5). It can be seen that both have a linear relationship with the concentration. When the concentration is 2000 mg / liter or more, the absorbance is saturated and does not change. Therefore,
It is understood that the absorbance should be measured in the low concentration region and the transmittance should be measured in the high concentration region.
【図１】本発明にかかる装置の構成例を示す図。FIG. 1 is a diagram showing a configuration example of an apparatus according to the present invention.
【図２】実施例１の結果を示す図FIG. 2 is a diagram showing the results of Example 1.
【図３】実施例１の結果を示す図FIG. 3 is a diagram showing the results of Example 1.
【図４】実施例１の結果を示す図FIG. 4 is a diagram showing the results of Example 1.
【図５】実施例１の結果を示す図FIG. 5 is a diagram showing the results of Example 1.
１：光源 ２：光照射ライン ３：受光ライン ４：入射光強度測定ライン ５：バンドパスフィルター ６：光センサー ７：薬液槽 ８：ギャップ 1: Light source 2: Light irradiation line 3: Light receiving line 4: Incident light intensity measurement line 5: Bandpass filter 6: Optical sensor 7: Chemical solution tank 8: Gap
Claims (4)
方法であって、溶液の吸光度または透過率を測定して濃
度を検知し管理することを特徴とする濃度管理方法。1. A method for controlling the concentration of a chemical solution that is circulated and used in a chemical solution tank, which comprises measuring the absorbance or transmittance of the solution to detect and control the concentration.
と、または測定波長を変更することにより測定感度を変
更することを特徴とする請求項１記載の方法。2. The method according to claim 1, wherein the measurement sensitivity is changed by adjusting the distance between the light irradiation unit and the light receiving unit, or by changing the measurement wavelength.
末端にピックアップレンズを有する光照射部、受光ピッ
クアップレンズと光ファイバーとからなる受光部、光源
からの光強度および受光部で検出された光強度を測定す
る光センサー、並びに前記光強度から吸光度または透過
率を得るためのコンピューターを有する薬液の濃度測定
装置。3. A light source, a light emitting section having an optical fiber connected to the light source and a pickup lens at an end, a light receiving section comprising a light receiving pickup lens and an optical fiber, a light intensity from the light source and a light intensity detected by the light receiving section. A concentration measuring device for a drug solution, comprising an optical sensor for measurement, and a computer for obtaining the absorbance or the transmittance from the light intensity.
とにより、または測定波長を変更することにより測定感
度を変更することを特徴とする請求項３記載の装置。4. The apparatus according to claim 3, wherein the measurement sensitivity is changed by adjusting the distance between the light irradiation unit and the light receiving unit or by changing the measurement wavelength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4320282A JP3055082B2 (en) | 1992-11-30 | 1992-11-30 | Concentration management method and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4320282A JP3055082B2 (en) | 1992-11-30 | 1992-11-30 | Concentration management method and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06167449A true JPH06167449A (en) | 1994-06-14 |
| JP3055082B2 JP3055082B2 (en) | 2000-06-19 |
Family
ID=18119768
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4320282A Expired - Fee Related JP3055082B2 (en) | 1992-11-30 | 1992-11-30 | Concentration management method and device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3055082B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002343987A (en) * | 2001-05-15 | 2002-11-29 | Showa Shell Sekiyu Kk | Manufacturing method for heterojunction thin film solar battery |
| JPWO2008105146A1 (en) * | 2007-02-28 | 2010-06-03 | サントリーホールディングス株式会社 | Liquid-type absorbance sensor element and absorptiometer using the same |
| WO2016079797A1 (en) * | 2014-11-18 | 2016-05-26 | 日本メクトロン株式会社 | Inline concentration measurement probe and concentration measurement system |
| CN107533004A (en) * | 2015-05-29 | 2018-01-02 | 尼普洛株式会社 | Transmitted intensity determination unit |
| JP2021043794A (en) * | 2019-09-12 | 2021-03-18 | 能美防災株式会社 | Separate type fire detector |
| US11610467B2 (en) | 2020-10-08 | 2023-03-21 | Ecolab Usa Inc. | System and technique for detecting cleaning chemical usage to control cleaning efficacy |
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| JPWO2008105146A1 (en) * | 2007-02-28 | 2010-06-03 | サントリーホールディングス株式会社 | Liquid-type absorbance sensor element and absorptiometer using the same |
| JP2012255806A (en) * | 2007-02-28 | 2012-12-27 | Suntory Holdings Ltd | Absorptiometer using liquid immersion type absorbance sensor element |
| WO2016079797A1 (en) * | 2014-11-18 | 2016-05-26 | 日本メクトロン株式会社 | Inline concentration measurement probe and concentration measurement system |
| CN107533004A (en) * | 2015-05-29 | 2018-01-02 | 尼普洛株式会社 | Transmitted intensity determination unit |
| JP2021043794A (en) * | 2019-09-12 | 2021-03-18 | 能美防災株式会社 | Separate type fire detector |
| US11610467B2 (en) | 2020-10-08 | 2023-03-21 | Ecolab Usa Inc. | System and technique for detecting cleaning chemical usage to control cleaning efficacy |
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