JP3352829B2 - Automatic preparation of dye solution - Google Patents
Automatic preparation of dye solutionInfo
- Publication number
- JP3352829B2 JP3352829B2 JP23037594A JP23037594A JP3352829B2 JP 3352829 B2 JP3352829 B2 JP 3352829B2 JP 23037594 A JP23037594 A JP 23037594A JP 23037594 A JP23037594 A JP 23037594A JP 3352829 B2 JP3352829 B2 JP 3352829B2
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- Japan
- Prior art keywords
- dye solution
- concentration
- dye
- tank
- solvent
- 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.)
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Description
【0001】[0001]
【産業上の利用分野】本発明は、色素溶液の自動調製方
法に関するものであり、詳しくは、色素溶液のスピンコ
ートプロセスにおける色素溶液の自動調製方法に関する
ものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for automatically preparing a dye solution, and more particularly to a method for automatically preparing a dye solution in a dye solution spin coating process.
【0002】[0002]
【従来の技術】近年、光導電、光電変換、発光、光記
録、表示などの各種の材料において、機能性有機色素を
利用した用途が拡大しており、品質や特性の維持、製品
歩留りの向上の観点から、コーティングプロセスにおけ
る色素溶液の濃度管理が益々重要となっている。2. Description of the Related Art In recent years, the use of functional organic dyes in various materials such as photoconductivity, photoelectric conversion, light emission, optical recording, and display has been expanding, maintaining quality and characteristics, and improving product yield. In view of this, it has become increasingly important to control the concentration of the dye solution in the coating process.
【0003】一方、色素コーティングの手法の一つにス
ピンコート法が知られているが、通常、スピンコートに
よる塗布を行う場合には、塗布液の殆どがスピンオフさ
れてしまうため、塗布液の製品への付着率は数%程度で
あり、回収された塗布液を再使用することが強く望まれ
ている。この場合、塗布時に回収された色素溶液は、溶
媒の蒸発により、濃度が上昇しているため、再使用に際
しては希釈操作が必要であり、そして、この希釈操作に
は、溶剤や洗浄時に回収された低濃度の色素溶液などを
利用することが出来る。[0003] On the other hand, a spin coating method is known as one of the dye coating techniques. However, when coating by spin coating, most of the coating liquid is usually spun off. The adhesion rate to the coating solution is about several percent, and it is strongly desired to reuse the recovered coating solution. In this case, since the concentration of the dye solution recovered at the time of application has increased due to evaporation of the solvent, a dilution operation is required when the dye solution is reused. For example, a low-concentration dye solution can be used.
【0004】[0004]
【発明が解決しようとする課題】しかしながら、上記の
希釈操作には、予め、各溶液の色素濃度を測定して各溶
液の混合比率を求める必要があるが、上記の回収色素溶
液の濃度は、常に一定ではないため、希釈操作は、必ず
しも容易ではない。本発明は、斯かる実情に鑑みなされ
たものであり、その目的は、スピンコートプロセスにお
ける色素溶液の濃度管理を適切に行い且つ色素の利用効
率を高めることを可能にする、色素溶液の自動調製方法
を提供することにある。However, in the above-mentioned dilution operation, it is necessary to measure the dye concentration of each solution in advance to determine the mixing ratio of each solution. The dilution operation is not always easy because it is not always constant. The present invention has been made in view of such circumstances, and an object of the present invention is to automatically control the concentration of a dye solution in a spin coating process and to enhance the efficiency of using the dye, thereby automatically preparing a dye solution. It is to provide a method.
【0005】[0005]
【課題を解決するための手段】すなわち、本発明の要旨
は、色素溶液のスピンコートプロセスにおける色素溶液
の調製方法であって、塗布時にスピンコーターから回収
された色素溶液のための回収タンク(A)と、溶剤タン
ク(B)及び/又はスピンコーターの洗浄時に回収され
た色素溶液のための洗浄廃液タンク(C)と、これらの
タンクから所定量の色素溶液および溶剤が供給されるロ
ードセル付濃度調整タンク(E)とを備え、濃度調整タ
ンク(E)で調製される色素溶液の濃度および重量を自
動測定すると共に、回収タンク(A)と溶剤タンク
(B)及び/又は洗浄廃液タンク(C)の色素溶液の色
素濃度を自動測定し、これらの測定値に基づき、濃度調
整タンク(E)で調製される色素溶液の濃度が目標値と
なる様に上記の各タンクから濃度調整タンク(E)に供
給される色素溶液および/または溶剤の重量を調整する
ことを特徴する色素溶液の自動調製方法に存する。That is, the gist of the present invention is a method for preparing a dye solution in a spin coating process of a dye solution, wherein a collection tank (A) for the dye solution collected from a spin coater at the time of coating is provided. ), A washing waste tank (C) for the dye solution collected during washing of the solvent tank (B) and / or the spin coater, and a concentration with a load cell to which a predetermined amount of the dye solution and the solvent are supplied from these tanks. A concentration tank (E) for automatically measuring the concentration and the weight of the dye solution prepared in the concentration adjustment tank (E), and a collection tank (A), a solvent tank (B), and / or a washing waste liquid tank (C). )), The dye concentrations of the dye solutions prepared above are automatically measured based on the measured values, and the concentrations of the dye solutions prepared in the concentration adjusting tank (E) are adjusted to the target values. It consists in the automatic preparation of a dye solution, characterized in that adjusting the weight of the dye solution and / or solvent is fed to the concentration adjusting tank (E) from.
【0006】以下、本発明の実施例を添付図面に基づい
て説明する。図1は、本発明の色素溶液の自動調製方法
を示す説明図であり、図2は、好ましい態様として使用
される色素溶液の濃度測定法において、カラム内に供給
された色素溶液試料が適正濃度に希釈されて吸光光度計
によって測定されるまでの過程を示す一例である。Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. FIG. 1 is an explanatory view showing an automatic method for preparing a dye solution according to the present invention. FIG. 2 shows a method for measuring the concentration of a dye solution used as a preferred embodiment. 1 is an example showing a process from dilution to measurement by an absorptiometer.
【0007】本発明の色素溶液の自動調製方法には、塗
布時にスピンコーターから回収された色素溶液のための
回収タンク(A)と、溶剤タンク(B)及び/又はスピ
ンコーターの洗浄時に回収された色素溶液のための洗浄
廃液タンク(C)と、これらのタンクから所定量の色素
溶液および溶剤が供給されるロードセル付濃度調整タン
ク(E)とを備えた設備を使用する。According to the method for automatically preparing a dye solution of the present invention, the recovery tank (A) for the dye solution recovered from the spin coater at the time of coating, and the recovery tank (B) and / or the recovery tank during cleaning of the spin coater are used. A facility comprising a washing waste liquid tank (C) for the prepared dye solution and a concentration adjusting tank (E) with a load cell to which a predetermined amount of the dye solution and solvent are supplied from these tanks is used.
【0008】回収タンク(A)に供給される色素溶液
は、溶媒の蒸発により、スピンコーターに供給される塗
布用色素溶液よりも濃度が高くなっている。従って、色
素の析出防止および析出した色素の再溶解のため、回収
タンク(A)には攪拌機やジャケットヒータを設けるの
が好ましい。そして、回収タンク(A)における色素の
加熱溶解は、回収タンク(A)に温度センサー及び液量
センサー(図示せず)を配置し、後述の演算装置(2
0)及び制御用コントローラ(30)によって自動制御
するのが好ましい。The concentration of the dye solution supplied to the recovery tank (A) is higher than that of the coating dye solution supplied to the spin coater due to evaporation of the solvent. Therefore, it is preferable to provide a stirrer or a jacket heater in the recovery tank (A) in order to prevent the precipitation of the dye and to redissolve the deposited dye. The heating and dissolving of the dye in the collection tank (A) is performed by disposing a temperature sensor and a liquid amount sensor (not shown) in the collection tank (A),
0) and the controller (30) for automatic control.
【0009】溶剤タンク(B)の溶剤は、色素溶液の溶
媒と同じ溶剤であり、色素溶液の希釈やスピンコーター
の洗浄などに使用される。洗浄廃液は、洗浄廃液タンク
(C)に色素溶液として回収され、その色素濃度は、洗
浄に要した溶剤の量によって著しく変化するが、塗布用
色素溶液の濃度よりも低い場合には、希釈用溶液として
使用することが出来る。色素溶液タンク(D)は、本発
明においては、必要に応じて備えられ、スピンコートプ
ロセスに必要な塗布用色素溶液が収容されている。色素
溶液タンク(D)には、色素粉末投入用フィーダー(図
示せず)が設けられ、また、回収タンク(A)と同様
に、色素の自動加熱溶解のため、攪拌機やジャケットヒ
ータ等を設けるのが好ましい。濃度調整タンク(E)に
は、上記の各タンクから供給される色素溶液および溶剤
を混合するため、攪拌機が設けられている。The solvent in the solvent tank (B) is the same solvent as the solvent for the dye solution, and is used for diluting the dye solution and washing the spin coater. The washing waste liquid is collected as a dye solution in the washing waste tank (C), and the dye concentration varies significantly depending on the amount of the solvent required for washing. It can be used as a solution. In the present invention, the dye solution tank (D) is provided as needed, and stores a coating dye solution necessary for the spin coating process. The dye solution tank (D) is provided with a feeder (not shown) for feeding a dye powder, and similarly to the recovery tank (A), a stirrer or a jacket heater is provided for automatic heating and dissolution of the dye. Is preferred. The concentration adjusting tank (E) is provided with a stirrer for mixing the dye solution and the solvent supplied from each of the tanks.
【0010】色素溶液濃度の自動測定は、基本的には、
従来公知の方法と同様に吸光光度計を使用して行われる
が、正確に濃度を測定する場合は、測定波長における吸
光度の範囲が0.25〜0.75程度となる様に予め試
料溶液を希釈する必要がある。The automatic measurement of the dye solution concentration is basically performed by
The measurement is performed using an absorptiometer in the same manner as a conventionally known method. However, when the concentration is to be accurately measured, the sample solution is previously prepared so that the absorbance range at the measurement wavelength is about 0.25 to 0.75. Need to be diluted.
【0011】本発明においては、上記問題を解決するた
め、カラム(10)の一端側から一定量の色素溶液試料
を供給すると共に一定の供給速度で溶媒を供給し、カラ
ム(10)の他端側から連続的に流出する溶液中の色素
濃度を吸光光度計(11)によって測定し、当該測定値
と予め求められた検量線とに基づき色素濃度を算出する
濃度測定法を使用するのが好ましい。In the present invention, in order to solve the above-mentioned problem, a fixed amount of a dye solution sample is supplied from one end of the column (10), a solvent is supplied at a constant supply rate, and the other end of the column (10) is supplied. It is preferable to use a density measurement method in which the dye concentration in a solution that continuously flows out from the side is measured by an absorptiometer (11), and the dye concentration is calculated based on the measured value and a previously obtained calibration curve. .
【0012】上記の測定法は、液体クロマトグラフィー
と同様にカラムを巧みに利用した測定法であって、希釈
用溶媒の連続した流れの中に一定微少量の色素溶液を注
入し、希釈用溶媒の流れの作用により、色素溶液を溶媒
中に混合・拡散させて希釈することを特徴とする。The above-mentioned measurement method is a measurement method utilizing a column similarly to liquid chromatography, in which a small amount of a dye solution is injected into a continuous flow of a solvent for dilution, and the solvent for dilution is used. The method is characterized in that the dye solution is mixed and diffused in a solvent to be diluted by the action of the flow of.
【0013】カラム(10)の形式としては、通常は、
空筒カラムが好適に使用されるが、色素の分解を惹起し
たり不均一な滞留がない限り特に制限されず、例えば、
テフロンビース等を充填したカラムを使用し、色素溶液
の溶媒中への混合・拡散を促進することも出来る。The format of the column (10) is usually
Although an empty column is suitably used, it is not particularly limited as long as it causes decomposition of the dye or non-uniform retention, for example,
By using a column filled with Teflon beads or the like, mixing and diffusion of the dye solution into the solvent can be promoted.
【0014】そして、カラム(10)の内径および長さ
は、色素溶液中の色素濃度によって適宜選択されるが、
通常、内径は1〜5mmの範囲から選択され、長さは3
0〜500mmの範囲から選択される。また、カラム
(10)としては、ステンレスカラム、ガラスカラム等
の各種のカラムを使用することが出来る。The inner diameter and length of the column (10) are appropriately selected depending on the dye concentration in the dye solution.
Usually, the inner diameter is selected from the range of 1 to 5 mm and the length is 3
It is selected from the range of 0 to 500 mm. As the column (10), various columns such as a stainless steel column and a glass column can be used.
【0015】カラム(10)への色素溶液試料の供給
は、試料インジェクター(12)と多方切替え弁(1
3)との共同作業によって行われる。すなわち、試料イ
ンジェクター(12)中に試料を流通させて多方切替え
弁(13)の流路を切り換えることにより、試料インジ
ェクター(12)中に一定量の試料を採取し、多方切替
え弁(13)の流路を切り換えることにより、溶媒供給
ポンプ(14)から連続供給される溶媒によって試料を
カラム(10)に供給する。試料インジェクター(1
2)の容量は、試料中の色素濃度、カラム(10)の内
径および長さ等によって異なるが、通常は0.1〜10
マイクロリットルの範囲から適宜選択される。The supply of the dye solution sample to the column (10) is performed by the sample injector (12) and the multi-way switching valve (1).
This is done in collaboration with 3). That is, by flowing the sample through the sample injector (12) and switching the flow path of the multi-way switching valve (13), a fixed amount of sample is collected in the sample injector (12), and the multi-way switching valve (13) is operated. By switching the flow path, the sample is supplied to the column (10) by the solvent continuously supplied from the solvent supply pump (14). Sample injector (1
The volume of 2) varies depending on the dye concentration in the sample, the inner diameter and length of the column (10), etc.
It is appropriately selected from the range of microliter.
【0016】溶媒供給ポンプ(14)としては、液体ク
ロマトグラフィー等で一般に使用されている定容量ポン
プが使用される。カラム(10)中において、色素溶液
は、溶媒の流れの作用によって混合・拡散されて希釈さ
れる。その結果、図2に示す様に、カラム(10)の一
端側(a)から供給された色素溶液の濃度は、カラム
(10)の他端側(b)に近付くに従い漸次低下させら
れる。As the solvent supply pump (14), a constant volume pump generally used in liquid chromatography or the like is used. In the column (10), the dye solution is mixed and diffused and diluted by the action of the solvent flow. As a result, as shown in FIG. 2, the concentration of the dye solution supplied from one end (a) of the column (10) gradually decreases as it approaches the other end (b) of the column (10).
【0017】カラム(10)の他端側(b)から連続的
に流出する試料中の濃度は、吸光光度計(11)によっ
て測定される。本発明において、カラム(10)の他端
側(b)から流出する溶液中の色素濃度は、測定波長光
における吸光度の範囲が0.2〜1.5程度となる様に
調整するのが好ましく、特に高度の測定精度を必要とす
る場合は、0.25〜0.75程度となる様に調整する
のが好ましい。The concentration in the sample continuously flowing out from the other end (b) of the column (10) is measured by an absorptiometer (11). In the present invention, the dye concentration in the solution flowing out from the other end (b) of the column (10) is preferably adjusted so that the range of absorbance at the measurement wavelength light is about 0.2 to 1.5. In particular, when a high degree of measurement accuracy is required, it is preferable to adjust the value to be about 0.25 to 0.75.
【0018】測定波長は、色素の光吸収波長領域の中か
ら、吸収スペクトルの形状と吸光度値とを考量して適宜
選択されるが、通常は、色素の吸収極大波長に設定され
る。また、複数の波長測定を行うことにより、濃度測定
の精度向上、溶液中の色素劣化の有無の確認、溶液中の
不純物の管理、混合色素溶液の色素毎の濃度測定などが
可能となる。なお、色素溶液中に例えば色素安定剤など
の添加剤が含まれている場合は、吸光光度計(11)と
共に、示差屈折率検出器、蛍光検出器、電気化学検出
器、電気伝導検出器などを補助的に設け、これらの添加
剤の濃度を併せて測定してもよい。The measurement wavelength is appropriately selected from the light absorption wavelength region of the dye in consideration of the shape of the absorption spectrum and the absorbance value, and is usually set to the absorption maximum wavelength of the dye. Further, by performing a plurality of wavelength measurements, it becomes possible to improve the accuracy of the concentration measurement, confirm the presence or absence of dye deterioration in the solution, manage impurities in the solution, measure the concentration of each dye in the mixed dye solution, and the like. When an additive such as a dye stabilizer is contained in the dye solution, a differential refractive index detector, a fluorescence detector, an electrochemical detector, an electric conduction detector, etc., together with the absorptiometer (11). And the concentrations of these additives may be measured together.
【0019】演算装置(20)は、吸光光度計(11)
による測定値と予め求められた検量線とに基づき試料中
の色素濃度を算出する機能を有する。すなわち、吸光光
度計(11)によって測定される吸光度の積分値を算出
し、予め求められた検量線と比較し、色素濃度を算出す
る。検量線は、複数種類の既知濃度の試料を使用するこ
とにより容易に求めることが出来る。The arithmetic unit (20) is an absorptiometer (11)
Has the function of calculating the dye concentration in the sample based on the measurement value obtained by the above and the calibration curve obtained in advance. That is, the integrated value of the absorbance measured by the absorptiometer (11) is calculated and compared with a previously obtained calibration curve to calculate the dye concentration. The calibration curve can be easily obtained by using a plurality of types of samples having known concentrations.
【0020】回収タンク(A)、溶剤タンク(B)、洗
浄廃液タンク(C)、色素溶液タンク(D)及び濃度調
整タンク(E)には、それぞれ、ポンプ(1)が備えら
れ、濃度調整タンク(E)を除く各タンクの流路には、
フイルター(2)及び開閉バルブ(3)が備えられ、更
に、回収タンク(A)、洗浄廃液タンク(C)及び色素
溶液タンク(D)の各流路には、流路切替えバルブ
(4)が備えられている。なお、密閉加圧タイプのタン
クを使用することにより、ポンプに代え、加圧力にて送
液を行うことも可能である。Each of the recovery tank (A), the solvent tank (B), the washing waste liquid tank (C), the dye solution tank (D) and the concentration adjusting tank (E) is provided with a pump (1). In the flow path of each tank except tank (E),
A filter (2) and an opening / closing valve (3) are provided, and a flow path switching valve (4) is provided in each flow path of the recovery tank (A), the washing waste liquid tank (C), and the dye solution tank (D). Provided. In addition, by using a closed pressurized type tank, it is also possible to perform liquid sending by pressurized force instead of a pump.
【0021】濃度調整タンク(E)の色素溶液濃度は、
次の様にして自動測定される。すなわち、色素溶液は、
ポンプ(1)により、試料インジェクター(12)に供
給され且つ多方切替え弁(13)の切替え操作によって
一定量採取されてカラム(10)に供給される。そし
て、前述の方法に従って濃度の自動測定が行われる。試
料インジェクター(12)からのドレンは、適宜、回収
タンク(A)、洗浄廃液タンク(C)、濃度調整タンク
(E)又は廃液タンク(図示せず)に回収される。The concentration of the dye solution in the concentration adjusting tank (E) is
It is automatically measured as follows. That is, the dye solution is
The pump (1) supplies the sample to the sample injector (12), and a certain amount is collected by the switching operation of the multi-way switching valve (13) and supplied to the column (10). Then, automatic measurement of the concentration is performed according to the above-described method. The drain from the sample injector (12) is appropriately collected in a collection tank (A), a washing waste liquid tank (C), a concentration adjusting tank (E), or a waste liquid tank (not shown).
【0022】回収タンク(A)、洗浄廃液タンク(C)
及び色素溶液タンク(D)の色素溶液濃度は、次の様に
して自動測定される。すなわち、各色素溶液は、試料切
替えバルブ(15)に供給され、その切替え操作によっ
て何れか一つの試料が試料インジェクター(12)に供
給され且つ多方切替え弁(13)の切替え操作によって
一定量採取されてカラム(10)に供給される。そし
て、前述の方法に従って濃度の自動測定が行われる。試
料インジェクター(12)からのドレンは、各色素溶液
の供給元タンク又は廃液タンク(図示せず)に回収され
る。Recovery tank (A), washing waste liquid tank (C)
The concentration of the dye solution in the dye solution tank (D) is automatically measured as follows. That is, each dye solution is supplied to the sample switching valve (15), and one of the samples is supplied to the sample injector (12) by the switching operation, and a fixed amount is collected by the switching operation of the multi-way switching valve (13). And supplied to the column (10). Then, automatic measurement of the concentration is performed according to the above-described method. Drain from the sample injector (12) is collected in a supply source tank or a waste liquid tank (not shown) of each dye solution.
【0023】スタートアップにおいては、例えば、上記
の各タンクの色素溶液の濃度を測定し、当該結果に基づ
き、所定濃度の色素溶液を調製するのに必要な混合比率
を計算し、当該結果に基づき、回収タンク(A)の色素
溶液と溶剤タンク(B)の溶剤および/または洗浄廃液
タンク(C)の色素溶液の所定量を濃度調整タンク
(E)に供給する。In the start-up, for example, the concentration of the dye solution in each of the above-mentioned tanks is measured, and based on the result, a mixing ratio required to prepare a dye solution having a predetermined concentration is calculated, and based on the result, A predetermined amount of the dye solution in the recovery tank (A), the solvent in the solvent tank (B) and / or the dye solution in the cleaning waste liquid tank (C) is supplied to the concentration adjusting tank (E).
【0024】そして、濃度調整タンク(E)で調製され
る色素溶液の濃度および重量を自動測定し、当該結果に
基づき、濃度調整タンク(E)で調製される色素溶液の
濃度が目標値となる様に上記の各タンクから濃度調整タ
ンク(E)に供給される色素溶液および/または溶剤の
重量を制御する。色素溶液および/または溶剤の重量の
計算は、演算装置(20)により、供給量の制御は、制
御用コントローラ(30)によって行われる。Then, the concentration and weight of the dye solution prepared in the concentration adjusting tank (E) are automatically measured, and based on the result, the concentration of the dye solution prepared in the concentration adjusting tank (E) becomes a target value. In this manner, the weight of the dye solution and / or the solvent supplied from each of the tanks to the density adjusting tank (E) is controlled. The calculation of the weight of the dye solution and / or the solvent is performed by the arithmetic unit (20), and the supply amount is controlled by the control controller (30).
【0025】すなわち、目標値、自動測定のインターバ
ル、各測定データ等は、演算装置(20)に入力され、
その出力信号に基づく制御用コントローラ(30)の指
令によりバルブ操作が行われ、濃度調整タンク(E)で
調製される色素溶液の濃度が一定値に維持される。上記
の各自動測定のインターバルは、濃度調整タンク(E)
の色素溶液の濃度変化の程度などを考慮して適宜設定さ
れる。そして、濃度調整タンク(E)で調製される色素
溶液の重量の自動測定は、当該タンクに設置されたロー
ドセル(40)により行われる。That is, a target value, an automatic measurement interval, each measurement data, and the like are input to the arithmetic unit (20).
A valve operation is performed according to a command from the control controller (30) based on the output signal, and the concentration of the dye solution prepared in the concentration adjusting tank (E) is maintained at a constant value. The interval of each of the above automatic measurements is the concentration adjustment tank (E)
Is appropriately set in consideration of the degree of change in the concentration of the dye solution. The automatic measurement of the weight of the dye solution prepared in the concentration adjusting tank (E) is performed by a load cell (40) installed in the tank.
【0026】また、スピンコートに伴い、全体の色素量
は徐々に消費されて減少する。このため、演算装置(2
0)において、各タンクの色素濃度および重量の測定値
に基づいた全色素量を管理させ、必要に応じ、色素溶液
タンク(D)にて調製された色素溶液を濃度調整タンク
(E)に供給して補うことが出来る。この場合、色素溶
液タンク(D)の色素溶液の濃度および濃度調整タンク
(E)への供給量は、他のタンクの色素溶液の場合と同
様に演算装置(20)に入力される。こうして、濃度調
整タンク(E)で濃度調整された色素溶液は、スピンコ
ートプロセスに安定して供給される。Further, with the spin coating, the total amount of the dye is gradually consumed and decreased. Therefore, the arithmetic unit (2
In 0), the total amount of the dye is controlled based on the measured values of the dye concentration and the weight of each tank, and the dye solution prepared in the dye solution tank (D) is supplied to the concentration adjusting tank (E) as necessary. You can make up for it. In this case, the concentration of the dye solution in the dye solution tank (D) and the amount supplied to the concentration adjusting tank (E) are input to the arithmetic unit (20) in the same manner as in the case of the dye solutions in the other tanks. Thus, the dye solution whose concentration has been adjusted in the concentration adjusting tank (E) is stably supplied to the spin coating process.
【0027】[0027]
【実施例】以下、本発明を実施例に基づき更に詳細に説
明するが、本発明は、その要旨を超えない限り、以下の
実施例に限定されるものではない。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist.
【0028】実施例1 光記録媒体の製造におけるスピンコートプロセスにおい
て、複数基のスピンコータを使用して、(i)色素溶液
の基板への塗布とスピンコーターからの色素溶液の回
収、(ii)スピンコータの洗浄と洗浄廃液の回収の各工程
を各スピンコータ毎に順次に繰り返し実施し、複数基の
スピンコーターの上記(i)及び(ii)の各工程から排出
される色素溶液を回収した。Example 1 In a spin coating process in the production of an optical recording medium, using a plurality of spin coaters, (i) applying a dye solution to a substrate and collecting the dye solution from the spin coater, and (ii) spin coater The steps of washing and collecting the washing waste liquid were sequentially and repeatedly performed for each spin coater, and the dye solutions discharged from the above steps (i) and (ii) of the plurality of spin coaters were collected.
【0029】基板への塗布には、日本感光色素(株)製
の色素「NK−3663」とメタノール溶媒とから成る
濃度1.0重量%の色素溶液を使用し、スピンコータの
洗浄には、溶剤タンク(B)に収容されたメタノールを
使用した。塗布時にスピンコーターから回収された色素
溶液は、回収タンク(A)に連続的に供給し、洗浄時に
スピンコーターから回収された色素溶液は、洗浄廃液タ
ンク(C)に連続的に供給した。そして、上記の回収色
素溶液を使用し、図1に示す方法に従って以下の様に色
素溶液の自動調整を行った。A 1.0% by weight dye solution comprising a dye "NK-3663" manufactured by Nippon Kogaku Dye Co., Ltd. and a methanol solvent was used for coating on the substrate. The methanol contained in the tank (B) was used. The dye solution recovered from the spin coater during coating was continuously supplied to the recovery tank (A), and the dye solution recovered from the spin coater during cleaning was continuously supplied to the cleaning waste liquid tank (C). Then, using the recovered dye solution, the dye solution was automatically adjusted as follows in accordance with the method shown in FIG.
【0030】回収タンク(A)及び洗浄廃液タンク
(C)の各色素溶液は、各タンクに備えられたポンプ
(1)、フイルター(2)、開閉バルブ(3)及び流路
切替えバルブ(4)を通してロードセル付濃度調整タン
ク(E)に供給されると共に流路切替えバルブ(4)の
切替え操作によって濃度の自動測定に供された。一方、
溶剤タンク(B)のメタノールは、タンクに備えられた
ポンプ(1)、フイルター(2)及び開閉バルブ(3)
を通してロードセル付濃度調整タンク(E)に供給され
た。Each dye solution in the recovery tank (A) and the washing waste liquid tank (C) is supplied to a pump (1), a filter (2), an opening / closing valve (3) and a flow path switching valve (4) provided in each tank. And supplied to the concentration adjusting tank (E) with a load cell, and the concentration was automatically measured by switching the flow path switching valve (4). on the other hand,
The methanol in the solvent tank (B) is supplied to a pump (1), a filter (2) and an opening / closing valve (3) provided in the tank.
To the concentration adjusting tank with load cell (E).
【0031】上記の濃度の自動測定は、試料切替えバル
ブ(15)及び多方切替え弁(13)の自動切替え操作
により行われた。すなわち、定量ポンプ(14)によ
り、カラム(10)の一端側(a)から溶媒(クロロホ
ルム)が連続的に供給されて他端側(b)から連続的に
流出させられ、試料試料インジェクター(12)によ
り、カラム(10)の一端側(a)から、0.2マイク
ロリットルの色素溶液が注入された。そして、カラム
(10)の他端側(b)から連続的に流出する溶液の吸
光度の変化は、吸光光度計(11)に連続的に測定さ
れ、演算装置(20)に入力された。The automatic measurement of the concentration was carried out by an automatic switching operation of the sample switching valve (15) and the multi-way switching valve (13). That is, the solvent (chloroform) is continuously supplied from one end (a) of the column (10) and continuously discharged from the other end (b) by the metering pump (14). ), 0.2 microliter of the dye solution was injected from one end (a) of the column (10). Then, the change in the absorbance of the solution continuously flowing out from the other end side (b) of the column (10) was continuously measured by the absorptiometer (11) and input to the arithmetic unit (20).
【0032】吸光光度計(11)には、東ソー(株)製
の吸光光度計「UV−8010」を使用し、測定波長
は、色素の吸収極大波長である683nmに設定した。
また、演算装置(20)に予め入力された各濃度と吸光
度の積分値との関係(検量線)は、異なる濃度の色素溶
液を使用し、カラム(10)の他端側(b)から流出す
る溶液中の色素濃度が吸光度で0.25〜0.75の範
囲となる様に溶媒の供給速度を5ml/分に調整して求
めた。また、上記の濃度測定においても、カラム(1
0)の他端側(b)から流出する溶液中の色素濃度が吸
光度で0.25〜0.75の範囲となる様に溶媒の供給
速度を調整した。As the absorption photometer (11), an absorption photometer “UV-8010” manufactured by Tosoh Corporation was used, and the measurement wavelength was set to 683 nm, which is the maximum absorption wavelength of the dye.
In addition, the relationship (calibration curve) between each concentration and the integrated value of absorbance previously input to the arithmetic unit (20) is obtained by using dye solutions of different concentrations and flowing out from the other end (b) of the column (10). The solvent supply rate was adjusted to 5 ml / min so that the dye concentration in the resulting solution was in the range of 0.25 to 0.75 in absorbance. In the above concentration measurement, the column (1
The supply rate of the solvent was adjusted such that the dye concentration in the solution flowing out from the other end side (b) of 0) was in the range of 0.25 to 0.75 in absorbance.
【0033】一方、濃度調整タンク(E)で調製される
色素溶液は、タンクに備えられたポンプ(1)により、
上記同様に濃度の自動測定に供された。すなわち、カラ
ム(10)の他端側(b)から連続的に流出する溶液の
吸光度の変化は、吸光光度計(11)で連続的に測定さ
れ、演算装置(20)に入力され、また、濃度調整タン
ク(E)で調製される色素溶液の重量は、ロードセル
(40)により自動測定され、演算装置(20)に入力
された。On the other hand, the dye solution prepared in the concentration adjusting tank (E) is supplied by a pump (1) provided in the tank.
It was subjected to the automatic measurement of the concentration in the same manner as described above. That is, the change in the absorbance of the solution continuously flowing out from the other end side (b) of the column (10) is continuously measured by the absorptiometer (11) and input to the arithmetic unit (20). The weight of the dye solution prepared in the concentration adjusting tank (E) was automatically measured by the load cell (40) and input to the arithmetic unit (20).
【0034】演算装置(20)からの出力に基づく制御
用コントローラー(30)の操作により、前記の各弁操
作による各色素溶液の自動濃度測定および濃度調整タン
ク(E)で調製される色素溶液の重量測定は、10分間
隔で実施され、各タンクから調整タンク(E)に供給さ
れる色素溶液およびメタノールの量が制御された。その
結果、各タンクから調整タンク(E)に供給される色素
溶液の濃度は常に変化するものの、調整タンク(E)で
調整された色素溶液の濃度は、目標値の濃度1.2重量
%に維持された。The operation of the control controller (30) based on the output from the arithmetic unit (20) allows the automatic concentration measurement of each dye solution by operating the above-mentioned respective valves, and the measurement of the dye solution prepared in the concentration adjusting tank (E). The weight measurements were performed at 10 minute intervals, and the amounts of the dye solution and methanol supplied from each tank to the adjustment tank (E) were controlled. As a result, although the concentration of the dye solution supplied from each tank to the adjustment tank (E) constantly changes, the concentration of the dye solution adjusted in the adjustment tank (E) is reduced to the target concentration of 1.2% by weight. Maintained.
【0035】[0035]
【発明の効果】以上説明した本発明によれば、スピンコ
ートプロセスにおける色素溶液の濃度管理を適切に行い
且つ色素の利用効率を高めることを可能にする、色素溶
液の自動調製方法が提供される。本発明に係る色素溶液
の自動調製方法は、例えば、記録層に有機色素を利用し
たライトワンス型光記録デイスクの安価な製造方法に寄
与することが出来る。According to the present invention described above, there is provided a method for automatically preparing a dye solution, which makes it possible to appropriately control the concentration of the dye solution in the spin coating process and to increase the use efficiency of the dye. . The method for automatically preparing a dye solution according to the present invention can contribute, for example, to an inexpensive method for producing a write-once optical recording disk using an organic dye for the recording layer.
【図1】本発明の色素溶液の調製方法を示す説明図であ
る。FIG. 1 is an explanatory diagram showing a method for preparing a dye solution of the present invention.
【図2】カラム内に供給された色素溶液試料が適正濃度
に希釈されて吸光光度計によって測定されるまでの過程
を示す一例である。FIG. 2 is an example showing a process until a dye solution sample supplied to a column is diluted to an appropriate concentration and measured by an absorptiometer.
A:回収タンク B:溶剤タンク C:洗浄廃液タンク D:色素溶液タンク E:ロードセル付濃度調整タンク 10:カラム 11:吸光光度計 12:試料インジェクター 13:多方切替え弁 14:溶媒供給ポンプ 20:演算装置 30:制御用コントローラ 40:ロードセル A: Recovery tank B: Solvent tank C: Wash waste liquid tank D: Dye solution tank E: Concentration adjusting tank with load cell 10: Column 11: Absorbance meter 12: Sample injector 13: Multi-way switching valve 14: Solvent supply pump 20: Operation Device 30: Controller for control 40: Load cell
───────────────────────────────────────────────────── フロントページの続き (72)発明者 本田 卓生 神奈川県平塚市黒部丘1番31号 日本た ばこ産業株式会社 生産技術開発センタ ー内 (72)発明者 森田 真一 神奈川県横浜市緑区鴨志田町1000番地 三菱化成株式会社 総合研究所内 (56)参考文献 特開 昭63−111970(JP,A) 特開 平4−171038(JP,A) 特開 平5−255606(JP,A) 特開 昭48−39871(JP,A) 特開 平8−68748(JP,A) 特開 平6−190256(JP,A) 特開 平2−276830(JP,A) 特開 平6−204623(JP,A) 実開 昭62−10438(JP,U) (58)調査した分野(Int.Cl.7,DB名) B05D 1/40 B05D 3/00 G11B 7/26 B05C 11/10 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Takuo Honda 1-31 Kurobeoka, Hiratsuka-shi, Kanagawa Japan Tobacco Inc. Production Technology Development Center (72) Inventor Shinichi Morita Midori-ku, Yokohama-shi, Kanagawa No. 1000 Kamoshida-cho Mitsubishi Research Institute, Ltd. (56) References JP-A-63-111970 (JP, A) JP-A-4-171038 (JP, A) JP-A-5-255606 (JP, A) JP-A-48-39871 (JP, A) JP-A-8-68748 (JP, A) JP-A-6-190256 (JP, A) JP-A-2-276830 (JP, A) JP-A-6-204623 (JP JP, A) Japanese Utility Model Sho 62-10438 (JP, U) (58) Fields investigated (Int. Cl. 7 , DB name) B05D 1/40 B05D 3/00 G11B 7/26 B05C 11/10
Claims (2)
る色素溶液の調製方法であって、塗布時にスピンコータ
ーから回収された色素溶液のための回収タンク(A)
と、溶剤タンク(B)及び/又はスピンコーターの洗浄
時に回収された色素溶液のための洗浄廃液タンク(C)
と、これらのタンクから所定量の色素溶液および溶剤が
供給されるロードセル付濃度調整タンク(E)とを備
え、濃度調整タンク(E)で調製される色素溶液の濃度
および重量を自動測定すると共に、回収タンク(A)と
溶剤タンク(B)及び/又は洗浄廃液タンク(C)の色
素溶液の色素濃度を自動測定し、これらの測定値に基づ
き、濃度調整タンク(E)で調製される色素溶液の濃度
が目標値となる様に上記の各タンクから濃度調整タンク
(E)に供給される色素溶液および/または溶剤の重量
を制御することを特徴とする色素溶液の自動調製方法。1. A method for preparing a dye solution in a dye solution spin coating process, comprising: a collection tank (A) for a dye solution collected from a spin coater at the time of coating.
And a washing waste liquid tank (C) for the dye solution collected during washing of the solvent tank (B) and / or the spin coater.
And a concentration adjusting tank (E) with a load cell to which a predetermined amount of the dye solution and the solvent are supplied from these tanks. The concentration and weight of the dye solution prepared in the concentration adjusting tank (E) are automatically measured and The dye concentration of the dye solution in the recovery tank (A), the solvent tank (B), and / or the washing waste liquid tank (C) is automatically measured, and the dye prepared in the concentration adjusting tank (E) based on these measured values. A method for automatically preparing a dye solution, comprising controlling the weight of the dye solution and / or the solvent supplied from each of the above-mentioned tanks to the concentration adjusting tank (E) so that the concentration of the solution becomes a target value.
料を供給すると共に一定の供給速度で溶媒を供給し、カ
ラムの他端側から連続的に流出する溶液中の色素濃度を
吸光光度計によって測定し、当該測定値と予め求められ
た検量線とに基づき色素濃度を算出する色素溶液の濃度
測定法を使用する請求項1に記載の色素溶液の自動調製
方法。2. An absorptiometer that supplies a fixed amount of a dye solution sample from one end of a column, supplies a solvent at a constant supply rate, and measures the dye concentration in a solution continuously flowing out from the other end of the column. 2. A method for automatically preparing a dye solution according to claim 1, wherein a dye solution concentration measurement method is used, wherein the dye concentration is calculated based on the measured value and a calibration curve obtained in advance.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP23037594A JP3352829B2 (en) | 1994-08-31 | 1994-08-31 | Automatic preparation of dye solution |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP23037594A JP3352829B2 (en) | 1994-08-31 | 1994-08-31 | Automatic preparation of dye solution |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH0871494A JPH0871494A (en) | 1996-03-19 |
JP3352829B2 true JP3352829B2 (en) | 2002-12-03 |
Family
ID=16906884
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JP23037594A Expired - Lifetime JP3352829B2 (en) | 1994-08-31 | 1994-08-31 | Automatic preparation of dye solution |
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JP (1) | JP3352829B2 (en) |
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JP3880268B2 (en) * | 2000-01-28 | 2007-02-14 | 松下電器産業株式会社 | Recycling method of adhesive used for laminating discs |
FI109926B (en) * | 2001-04-20 | 2002-10-31 | Valmet Raisio Oy | Method and system for controlling the coating recipe |
JP3924134B2 (en) * | 2001-05-18 | 2007-06-06 | 富士フイルム株式会社 | Manufacturing method of optical information recording medium |
JP2003272245A (en) * | 2002-03-14 | 2003-09-26 | Ricoh Co Ltd | Method for manufacturing optical recording medium |
JP5898895B2 (en) * | 2011-09-27 | 2016-04-06 | 積水化学工業株式会社 | Solution concentration adjusting method, solution concentration adjusting device, and method for producing dye-sensitized solar cell |
CN115228695B (en) * | 2022-05-24 | 2023-06-23 | 中材锂膜有限公司 | Solidification and water washing solution concentration quick adjustment system of lithium battery oil system coating diaphragm equipment |
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---|---|---|---|---|
JPS5521366B2 (en) * | 1971-09-23 | 1980-06-09 | ||
JPS6210438U (en) * | 1985-07-04 | 1987-01-22 | ||
JPS63111970A (en) * | 1986-10-27 | 1988-05-17 | Mitsubishi Electric Corp | Method for coating phosphor slurry |
JP2717697B2 (en) * | 1989-04-18 | 1998-02-18 | コニカ株式会社 | Method for producing cellulose triacetate film |
JPH04171038A (en) * | 1990-11-05 | 1992-06-18 | Kanebo Ltd | Apparatus for continuously supplying treatment solution with constant concentration |
JPH05255606A (en) * | 1992-03-13 | 1993-10-05 | Tdk Corp | Preparation of dye-containing. coating liquid |
JPH06190256A (en) * | 1992-12-28 | 1994-07-12 | Sumitomo Chem Co Ltd | Developer compounding device and developer compounding method |
JPH06204623A (en) * | 1992-12-28 | 1994-07-22 | Toshiba Corp | Coloring-matter-solution circulating apparatus |
JPH0868748A (en) * | 1994-08-31 | 1996-03-12 | Mitsubishi Chem Corp | Measurement of concentration of dye solution |
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1994
- 1994-08-31 JP JP23037594A patent/JP3352829B2/en not_active Expired - Lifetime
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JPH0871494A (en) | 1996-03-19 |
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