WO2007004612A1 - Procédé de production d'un substrat en régulant la concentration en matières organiques dans la solution de décapage - Google Patents

Procédé de production d'un substrat en régulant la concentration en matières organiques dans la solution de décapage Download PDF

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Publication number
WO2007004612A1
WO2007004612A1 PCT/JP2006/313234 JP2006313234W WO2007004612A1 WO 2007004612 A1 WO2007004612 A1 WO 2007004612A1 JP 2006313234 W JP2006313234 W JP 2006313234W WO 2007004612 A1 WO2007004612 A1 WO 2007004612A1
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WIPO (PCT)
Prior art keywords
concentration
substrate
tank
stripping
organic substance
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Application number
PCT/JP2006/313234
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English (en)
Japanese (ja)
Inventor
Takashi Tsuda
Masanao Sumita
Katsuyoshi Harada
Original Assignee
Toagosei Co., Ltd.
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Filing date
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Application filed by Toagosei Co., Ltd. filed Critical Toagosei Co., Ltd.
Priority to JP2007524056A priority Critical patent/JPWO2007004612A1/ja
Publication of WO2007004612A1 publication Critical patent/WO2007004612A1/fr

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Classifications

    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G03F7/42—Stripping or agents therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
    • H01L21/6704—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing

Definitions

  • the present invention relates to a stripping process in which a stripping solution is brought into contact with a coating material on a substrate to strip the coating material from the substrate, and a substrate material having at least a part of the coating material peeled off by the stripping step. And a removing step of removing a residue of an organic substance derived therefrom.
  • the present invention relates to a substrate manufacturing method capable of managing the organic residue on the substrate after the removal process.
  • Patent Document 1 Japanese Patent Laid-Open No. 2003-203856
  • Patent Document 2 JP 2003-330206 A
  • Patent Document 3 Japanese Patent Laid-Open No. 2003-305418
  • a cyclic carbonate having low reactivity with ozone is used as a stripping solution.
  • a stripping solution containing a dissolved organic material derived from the coating material hereinafter referred to as “dissolved organic material”
  • dissolved organic material a stripping solution containing a dissolved organic material derived from the coating material
  • Dissolved organic matter composed of a high molecular weight substance is converted into a low molecular compound by oxidative decomposition in an ozone treatment tank, and the stripping solution containing the low molecular weight compound is a stripping liquid for stripping and dissolving the coating material on the substrate again.
  • the low molecular weight compound has an extremely high limit concentration (hereinafter referred to as “acceptable concentration”) that adversely affects the stripping performance, compared to an organic material having a high molecular weight derived from an undegraded coating material. Therefore, even a stripping solution containing a low molecular compound at a high concentration can ensure stable and high stripping performance. As a result, the amount of stripping solution consumed can be greatly reduced, improving the economy and reducing the burden on the environment.
  • the concentration of the dissolved organic substance composed of a high molecular compound or the decomposed low molecular compound in the peeling liquid exceeds the allowable concentration, the peeling performance may be deteriorated, Contamination of the surface, that is, the coating substance residue on the surface of the substrate reattaches, resulting in defective products and a decrease in product yield.
  • the concentration of organic substances derived from the coating substance was measured by measuring the absorbance of ultraviolet rays, etc., and the concentration was controlled.
  • concentration control by absorbance measurement was not possible.
  • the present invention has been made in view of the above-described problems and problems, and a first object is to provide a peeling step in which the coating material on the substrate is brought into contact with the coating liquid to separate the coating material from the substrate.
  • the organic substance derived from the coating substance from the substrate from which the coating substance has been peeled off at least partially by the peeling process A method for producing a substrate, which can manage organic residues on the substrate subjected to the removal step and improve the yield of the substrate. There is to do.
  • the second purpose is to produce a substrate that can also efficiently use the stripping solution, greatly reduce the consumption of the stripping solution, improve the economy, and reduce the burden on the environment. It is to provide a method.
  • the peeling step includes
  • the removal step includes
  • the residue of the organic matter on the substrate on which the removing step has been performed is not more than a predetermined control value.
  • a contact tank that receives a stripping solution in which the coating material is peeled off and an organic substance derived from the coating material is dissolved; a processing tank in which the stripping solution in which the organic matter is dissolved in the contact tank is used as the regenerative stripping solution;
  • a circulation type peeling device having The organic substance concentration in the stripping solution of the circulating stripping device is
  • Data on the inflow speed at which the organic matter dissolved in the stripping solution flows into the contact tank, data on the discharge speed of the stripping liquid discharged from the circulation type stripping device, and the stripping liquid is the contact tank force.
  • Data storage means storing data including outflow rate data flowing into the tank;
  • the organic matter concentration data in the contact tank, the inflow speed data, the discharge speed data, the outflow speed data, and the regenerative stripping solution are transferred from the treatment tank to the contact tank. From the data of the inflow velocity flowing into the tank and the data of the inflow velocity at which the newly replenished stripping liquid flows into the contact tank, the inside of the contact tank at the third time after a unit time has elapsed from the second time.
  • a concentration calculating means including a second concentration calculating means for calculating an organic substance concentration
  • the organic substance concentration in the contact tank at the third time is set as the organic substance concentration in the contact tank at the second time, and the organic substance concentration in the contact tank is Concentration calculating means for repeatedly calculating a predetermined number of times;
  • Output means for outputting a signal representing the organic substance concentration calculated by the concentration calculating means
  • FIG. 1 is a schematic view of a circulation type peeling device for explaining a first embodiment of the present invention.
  • FIG. 2 is a schematic configuration diagram of an organic matter concentration calculation apparatus applied to the first embodiment of the present invention.
  • FIG. 3 is a flow chart showing the procedure for calculating the organic substance concentration in the organic substance calculating means 300 of FIG.
  • FIG. 4 is a flowchart showing a procedure for causing a computer to execute a program applied to the first embodiment of the present invention.
  • FIG. 5 is a schematic diagram of another circulation type peeling apparatus applied to the first embodiment of the present invention.
  • FIG. 6 is a schematic view of a circulation type peeling apparatus for explaining a second embodiment of the present invention.
  • FIG. 7 is a schematic view of another circulation type peeling apparatus applied to the second embodiment of the present invention.
  • a step of performing a treatment for using a stripping solution in which an organic substance derived from the stripped coating material is dissolved as a reclaimed stripping solution, and a newly replenished stripping solution and regenerative stripping Removing the coating material from the substrate by bringing the liquid into contact with the coating material on the substrate, and a step of washing the surface of the substrate from which the coating material has been removed in the peeling step with water, and cleaning. And a removing step including drying the dried substrate with dry air.
  • the method for producing a substrate according to the present invention includes:
  • a stripping step in which a stripping solution is brought into contact with the coating material on the substrate to strip the coating material from the substrate, and a substrate force from which the coating material has been stripped at least partially by the stripping step is a residue of organic matter derived from the coating material. And a removing step for removing the substrate.
  • the peeling step includes
  • Including The removal step includes
  • the organic residue on the substrate on which the removal step has been performed is a predetermined control value or less.
  • a replenishing stripping solution is used to peel the coating material from the substrate by contacting the coating material on the substrate using the regenerative stripping solution. It can be very small. As a result, it becomes possible to use the stripping solution efficiently, and the consumption of the stripping solution can be greatly reduced, the economic efficiency can be improved, and the burden on the environment can be reduced.
  • the organic residue on the substrate after the removal step is below a predetermined control value, the number of organic residues on the substrate was adopted as the quality control standard of the substrate as a product. In this case, the product yield can be greatly improved, and continuous production is also possible within the quality control standards.
  • a contact tank that receives a peeling liquid in which the coating substance is peeled and an organic substance derived from the coating substance is dissolved, and a peeling liquid in which the organic substance in the contact tank is dissolved are used.
  • a circulation type stripping device having a treatment tank in which the processing to make a reclaimed stripping solution is used, and the organic matter concentration in the stripping solution of the circulating type stripping device is the inflow rate at which the organic matter dissolved in the stripping solution flows into the contact bath.
  • Data storage means for storing data including data, data on the discharge speed of the release liquid discharged from the circulation type peeling device, and data on the outflow speed at which the release liquid flows out from the contact tank to the treatment tank; At the first time, data on the concentration of organic matter in the contact tank, data on the inflow rate, data on the discharge rate, and data on the outflow rate
  • the first concentration calculating means for calculating the organic substance concentration in the contact tank at the second time after a unit time has elapsed from the first time, and the organic substance concentration data in the contact tank at the second time. Inflow rate data, discharge rate data, outflow rate data, inflow rate data where the regenerative stripping liquid flows from the treatment tank to the contact tank, and newly replenished stripping liquid into the contact tank.
  • a concentration calculation means including a second concentration calculation means for calculating an organic substance concentration in the contact tank at a third time after a unit time has elapsed from the second time, based on the inflow velocity data flowing in;
  • the organic substance concentration in the contact tank at the third time is set as the organic substance concentration in the contact tank at the second time, and the organic substance concentration in the contact tank is repeatedly calculated a predetermined number of times.
  • the calculation unit has an output unit that outputs a signal representing the organic substance concentration calculated by the calculation unit.
  • the concentration calculating means when calculating the concentration of the dissolved organic matter based on the stored data, the change in the concentration of the dissolved organic matter with the operation time after the start of peeling is complicated. It is possible to calculate the organic substance concentration easily and accurately without calculating based on the calculation of physical properties, and at the same time, it is possible to predict changes in the organic substance concentration.
  • stored data refers to data on the concentration of organic matter in the tank, data on the inflow rate at which organic matter dissolved in the stripping liquid flows into the contact tank, and stripping liquid is a circulating stripping device.
  • the discharge rate data of the stripping solution discharged from the tank, the outflow rate data from which the stripping solution flows out from the contact tank to the treatment tank, the inflow rate data from which the reclaimed stripping solution flows into the contact tank, and a new replenishment This is data such as the inflow rate at which the stripping solution flows into the contact tank, and is not limited to the data input and stored when calculating the organic substance concentration.
  • Stored data is also included. Therefore, it is not limited to the assumed value and may be an actual measurement value.
  • the production manager since it has data storage means, it can only predict changes in the organic matter concentration in the stripping solution when the assumed values such as the organic matter concentration data directly input from the keyboard touch panel etc. are stored. In addition, it can be used for process examination based on the predicted results, and even in various operating conditions, for example, when the type of substrate is changed, the production manager instructs simple and appropriate operating conditions. It becomes possible. On the other hand, when measured values of instrumentation equipment provided in the stripping device are input and stored, changes in the organic matter concentration in the stripping solution can be predicted even while the device is operating, and stripping is possible. It is easy to manage the stripping solution in the equipment.
  • the output means is provided, by providing a display device on the output means, the operator can visually recognize the change in the concentration of organic substances in the stripping solution, and can reduce the frequency of analysis and set up the work such as liquid removal. It is possible to improve work efficiency.
  • a recording medium such as paper or CDROM, it becomes easy to create operational instructions and refer to past calculation results.
  • the calculation device incorporates an organic concentration analyzer
  • concentration control with high accuracy becomes possible.
  • the substrate manufacturing method of the present invention it is possible to perform unattended operation of a circulation type peeling apparatus equipped with a calculation apparatus, and it is possible to fully automate.
  • the invention according to the present invention can also be applied to dissolution of a general organic film such as an oil film, a coating film, an organic contamination coating, and fine particles on the substrate.
  • a general organic film such as an oil film, a coating film, an organic contamination coating, and fine particles on the substrate.
  • the calculation device is a circulation type peeling device that performs processing for converting the organic substance concentration calculated by the concentration calculating means and the peeling liquid in which the organic substance derived from the coating substance is dissolved into a regenerative peeling liquid.
  • Correction coefficient storage means for storing the correction coefficient obtained based on the measured value of organic substance concentration at, and the concentration calculation means calculates the corrected organic substance concentration based on the calculated organic substance concentration and the correction coefficient. It is preferable to calculate the organic substance concentration in the contact tank and the treatment tank based on the corrected organic substance concentration.
  • the correction coefficient storage unit since the correction coefficient storage unit is provided, the calculation value of the organic substance concentration in the stripping solution is corrected to match the actual measurement value using a known method such as the least square method. Therefore, the correction coefficient can be identified and stored, and the correction coefficient can be stored in a database in advance within the condition range in which the apparatus can be manufactured. As a result, it is possible to easily determine the optimum operating conditions in consideration of productivity and economy by using a correction coefficient stored in a database for each type of substrate.
  • the organic substance concentration in the contact tank and in the treatment tank It is no longer necessary to calculate the organic substance concentration based on the calculation of physical properties just by making the calculation possible, and the organic substance concentration can be calculated easily and quickly.
  • the calculation apparatus further includes a control unit that controls an operation amount including a flow rate to the contact tank and the processing tank based on the output signal of the output unit force. .
  • the control means since the control means is provided, the operation amount such as the flow rate (inflow amount'outflow amount), pressure, temperature, etc. to the contact tank and the processing tank is controlled within the organic substance concentration management range. It becomes possible to automatically control the actual process. As a result, it is possible to manage the concentration of the organic matter simply and safely without relying on the intuition and experience of the equipment operator for changing the operating conditions and extending the life of the stripping solution.
  • the stripping solution contains ethylene carbonate as a main component, and in the stripping step, a stripping solution in which an organic substance derived from the stripped coating material is dissolved is used as a reclaimed stripping solution by ozone treatment.
  • the predetermined control value is 1.5 pieces / m 2 .
  • the substrate is managed by adopting a management value of 1.5 / m 2 regarding the residue of organic matter on the substrate on which the removal process has been performed as an evaluation standard for the manufactured substrate.
  • the productivity (yield) of the substrate which is a product, can be improved.
  • it if it is within the range of the control values adopted, it will be possible to operate the circulating stripper equipped with a calculation device unattended, and the stripping process can be fully automated.
  • a contact tank in which the coating substance is peeled off by contacting the coating substance on the substrate to dissolve in the peeling liquid as an organic substance derived from the coating substance, and a peeling liquid in which the organic substance in the contact tank is dissolved A program for causing a computer to calculate the concentration of organic substances in the stripping solution of a circulating stripping device having a treatment tank that is used as a recycled stripping solution.
  • the second unit time has elapsed from the first time.
  • the organic matter concentration data in the contact tank, the inflow speed data, the discharge speed data, the outflow speed data, and the regenerative stripping solution are transferred from the treatment tank to the contact tank.
  • Concentration of organic matter in the contact tank at the third time after the second time from the data of the inflow speed flowing into the tank and the data of the inflow speed at which the newly replenished stripping solution flows into the contact tank A second concentration calculation step for calculating The organic substance concentration in the contact tank at the third time is set as the organic substance concentration in the contact tank at the second time, and the organic substance concentration in the contact tank in the second concentration calculation step is repeatedly calculated a predetermined number of times. 3 concentration calculation steps;
  • the stripping solution is a cyclic carbonate or cyclic ester
  • the circulation type stripping device performs ozone treatment on the stripping solution in which the organic substance derived from the coating substance is dissolved in the processing tank, and stores it.
  • the calculated data includes a correction coefficient for correcting the calculated organic substance concentration to an actual measurement value of the organic substance concentration in the circulation type stripping apparatus that performs ozone treatment in the treatment tank, and calculates the organic substance concentration in the contact tank.
  • the peeling step is a step in which the coating material on the substrate is brought into contact with the stripping solution to strip the coating material from the substrate, and the stripping solution in which the organic material derived from the stripped coating material is dissolved is used.
  • a reclaimed stripper is treated, and the newly replenished stripper and reclaimed stripper are brought into contact with the coating material on the substrate to strip the coating material from the substrate.
  • the removal step is a step of removing organic residue derived from the coating material in addition to the strength of the substrate from which the coating material has been peeled off by the peeling step. In this process, the surface is washed with water, and the washed substrate is dried with dry air.
  • a coating material is peeled from the substrate by bringing a peeling solution into contact with the film material on the substrate using a circulation type peeling device.
  • FIG. 1 shows a schematic diagram of the circulation type peeling apparatus for explaining the present embodiment.
  • the circulation type peeling apparatus is also configured with a contact tank 10, an ozone treatment tank 20, a deaeration tank 30, a regenerated liquid tank 40, a new liquid tank 50, a contact chamber 60, and a force.
  • the contact tank 10 is a chamber for temporarily storing the stripping liquid flowing out from the chamber (when contact is made by nozzle supply) that performs the contact processing of the stripping liquid on the coating material coated on the substrate. It is. Further, the contact tank 10 may be a tank (in the case where the contact is by dipping) in which the stripping liquid is contacted with the coating material on the substrate. Furthermore, a plurality of contact tanks can be used in combination in order to ensure peeling of the coating substance from the substrate.
  • the peeling liquid is supplied from the nozzle to the surface of the organic film to form a liquid film of the peeling liquid.
  • the method of moving and moving is advantageous in terms of stripping speed.
  • nozzle force The amount of stripping solution supplied to the organic coating surface is determined by the balance between the capacity of the stripping device and the circulation rate of the stripping solution. Is also big.
  • ultrasonic waves are applied when the peeling liquid is brought into contact with the coating substance on the substrate.
  • the ozone treatment tank 20 is a tank for ozone treatment of the stripping solution after the contact treatment.
  • the ozone treatment is performed in the ozone treatment tank 20 and the regenerated stripping solution.
  • the amount of stripping solution used can be reduced, and the cost can be greatly reduced.
  • Typical examples of the stripping solution to which ozone treatment can be applied are organic compounds having a carbonate group or an ester group, and specifically, for example, ethylene carbonate, propylene carbonate, and ⁇ -butyrolatatone can be suitably used.
  • Tank 20 is provided separately and independently.
  • the degassing tank 30 is a tank that removes dissolved ozone in the liquid by publishing the effluent of the ozone treatment tank 20 with nitrogen gas or the like.
  • the regenerated liquid tank 40 is a tank for temporarily storing the regenerated stripping liquid from the deaeration tank 30.
  • the new liquid tank 50 is a tank that supplies pure stripping liquid to replenish the stripping liquid that has been consumed.
  • the flow of the stripping solution in the circulation type stripping apparatus is classified into three systems: a circulation system, an inflow system, and an outflow system.
  • the circulation system is a system in which a stripping solution containing a dissolved organic substance composed of a high molecular compound and a stripping solution in which an oxidatively decomposed low molecular weight compound is dissolved circulate.
  • a stripping solution containing a dissolved organic substance composed of a high molecular compound and a stripping solution in which an oxidatively decomposed low molecular weight compound is dissolved circulate.
  • it consists of ozone treatment tank 20, degassing tank 30, regenerated liquid tank 40, contact tank 10 and its connecting pipe, pump, ozone generator, etc. Is done.
  • the inflow system is a system in which the supply substance is supplied into the external force circulation system.
  • the supply substance is dissolved in the contact tank 1, and the pure organic substance supplied from the new liquid tank through the pipe.
  • the outflow system is a system in which substances flow out from the circulation system, and the outflow substances are the mist-like stripping liquid that is exhausted from the contact chamber 60 and the substrate after stripping by the stripping liquid in the contact chamber 60.
  • the outflow substances are the mist-like stripping liquid that is exhausted from the contact chamber 60 and the substrate after stripping by the stripping liquid in the contact chamber 60.
  • the temperature of the stripping solution in the contact tank 10 or the regenerating solution tank 40 is preferably kept high in order to maintain the more stable stripping performance, which is desirable from the viewpoint of stripping speed.
  • the preferred liquid temperature varies depending on the type of stripping solution, but when a polar organic solvent is used, 40 to 150 ° C is preferred, and 50 to 120 ° C is particularly preferred.
  • the peeling speed decreases, and when the liquid temperature is above the preferred liquid temperature range, the amount of the stripping liquid consumed increases due to an increase in the displacement, and the substrate is easily damaged.
  • the stripping solution temperature it is preferable to control the stripping solution temperature to 70 to 90 ° C in order to reduce organic residue derived from the coating substance. . This is because when the temperature is lower than 70 ° C, the peelability and solubility of the organic matter tend to decrease and the residue tends to increase. On the other hand, when the temperature exceeds 90 ° C, the metal film on the substrate is corroded. This is because the yield tends to decrease because the defect tends to increase and the number of defects tends to increase.
  • the temperature of the stripping solution in the ozone treatment tank 20 it is preferable to set the point of the solubility of ozone at a lower level than other tanks. Specifically, 20 to 100 ° C. is preferable, and 40 to 80 ° C. is particularly preferable.
  • the decomposition rate of acid-sodium decomposition by ozone for dissolved organic matter varies depending on the type of organic matter, it decomposes to low molecular weight compounds with a molecular weight of 100 or less when the decomposition proceeds sufficiently.
  • FIG. 2 is a schematic configuration diagram illustrating the entire organic substance concentration calculation apparatus according to the present embodiment.
  • this apparatus includes a data storage means 100, a correction coefficient storage means 200, a concentration calculation means 300, an output means 400, and a control means 500.
  • the data storage means 100 stores data on the concentration of organic matter in the tank, data on the inflow rate at which organic matter dissolved in the stripping solution flows into the contact bath, and the stripping solution from the contact bath.
  • These data are not limited to the data input and stored when calculating the organic substance concentration, but also include data already stored before the calculation. Therefore, these data are not limited to the assumed values. When assumed values such as organic substance concentration data directly input from keyboards, touch panels, etc., which are actually measured values, are stored.
  • the correction coefficient storage means 200 uses the ozone treatment tank 20 to perform the ozone treatment in the ozone treatment tank 20 by calculating the organic matter concentration in the stripping solution associated with the operation time after the start of stripping without considering complicated ozone decomposition.
  • a correction coefficient is stored for correction to match the measured value of the organic substance concentration in the circulation type stripping apparatus that has been subjected to. This is because when organic substances dissolved in the stripping solution are decomposed into low molecular weight compounds by ozone treatment, the organic molecules absorb oxygen due to oxidation, so the weight usually increases.
  • the amount of change in weight is calculated theoretically because it varies depending on the type of material, the degree of organic film modification (due to etching, ashing, ion implantation, etc.), and the conditions of ozone treatment (ozone concentration, treatment time, temperature, etc.) Have difficulty. Therefore, the organic substance concentration is calculated by correcting the organic substance concentration calculated based on a virtual process in which the ozone treatment is not performed by the concentration calculating means 300 described later using a correction coefficient.
  • the concentration calculation means 300 includes a first concentration calculation means 310 and a second calculation means 320 as shown in FIG.
  • the organic substance concentration can be calculated by calculating the mass balance of the stripping solution in the process in the circulation type stripping device. This calculation method will be described with reference to FIG. 3 which is a flowchart showing the organic substance concentration calculation by the concentration calculation means 300.
  • the amount of the stripping solution flowing in the circulation system is constant, so from FIG. 1, the amount of stripping solution containing dissolved organic matter per unit time flows into the contact tank 10 and the regeneration rate.
  • the stripping device force is also equal to the total amount of the stripping solution discharged and the amount of the stripping solution flowing from the contact tank 10 to the treatment tank 20.
  • the volume of the contact tank 10, the ozone treatment tank 20, the degassing tank 30, the regenerated liquid tank 40, and the new liquid tank 50 are set to VI, V2, V3, V4, and V5, respectively, and the organic matter concentration
  • the “%” is Dl, D2, D3, D4, D5
  • the inflow rate of organic matter dissolved in the stripper “71 ⁇ 11” is 1 ⁇
  • the outflow rate “LZmin” from the contact tank is S + R
  • the inflow rate of the newly replenished stripping solution “L The flow rate of the regenerative stripping solution is S + R “LZmin”, and the discharge rate to the outside of the device is R + L “LZmin”.
  • the organic substance concentration calculation in the concentration calculation means 300 is performed by the first concentration calculation means 310 when calculating by the initial value, and by the second concentration calculation means 320 when calculating thereafter.
  • the organic substance concentration in each tank can be calculated in the same way.
  • input data necessary for organic substance concentration calculation is read from the data storage means 100 and set as an initial value (S10).
  • the data to be read is the maximum calculation time, the volume of each tank: V1 to V5 “L”, the initial value “%” of the organic substance concentration D1 to D5 of each tank, the correction coefficient, and the peeling on the substrate.
  • the time t exceeds the maximum calculation time (Sl l). If it is determined that time t does not exceed the maximum calculation time (YES), unit time ⁇ is added to time t (S12), and organic matter concentrations D1 to D4 in each tank after unit time are calculated. (S13-S20).
  • the number of times of repeated calculation using the second concentration calculation means is (time until the maximum calculation time) Z (unit time) 2. For example, if the time until the maximum calculation time is ⁇ , the first concentration calculation means calculates the organic matter concentration in the tank at the second time when the unit time ⁇ has elapsed from the first time, and the repeated calculation is Not performed.
  • the concentration is calculated by the concentration calculation means 2 and is not repeated.
  • the second concentration meter is used to calculate the organic substance concentration in the tank at the time when the unit time ⁇ has passed since the time when the unit time ⁇ has passed since the third time. Repeat the calculation once using the calculation means.
  • the organic substance inflow amount A into the specified tank is calculated (S13).
  • the organic substance inflow A of the contact tank 10 can be calculated by R + D4 X (S + R + DZ100.
  • the organic substance outflow B of the specified tank is calculated (S14).
  • the organic matter effluent B can be calculated by Dl X ((S + R) + (R + L)) ZlOO, and then the organic matter increase C in the specified tank is calculated (S15).
  • the organic matter increase amount C can be calculated by A- B.
  • the organic matter concentration D in the identified tank is calculated (S16) .
  • the organic matter concentration D in the contact tank 10 is (the organic matter in the contact tank 10 at time t) Calculate as (concentration) + CX VI X 100.
  • the organic matter concentration is calculated to determine whether or not the tank is the ozone treatment tank 20 (S17). 0 When it is determined that the tank is the ozone treatment tank 20 (YES), the calculated organic matter is calculated. The density is corrected by the correction coefficient (S18). As a result, the organic substance concentration in the ozone treatment tank 20 after the ozone treatment can be calculated. Then proceed to S19. When it is determined that the tank is a tank other than the ozone tank 20 (NO), the process proceeds to S19.
  • the calculated value of the organic substance concentration in the identified tank is stored (S19). So After that, it is determined whether or not the organic substance concentration is calculated for all the tanks (S20). If it is determined that the organic matter concentration is being calculated for all tanks (YES), return to S11 to repeat the organic matter concentration calculation. When it is determined that there is a tank that has not been calculated (NO), the process returns to S13 for calculation for all the tanks.
  • the output unit 400 outputs a signal representing the organic substance concentration calculated by the concentration calculation unit 300. Therefore, by providing a display device in the output means, the operator can visually recognize changes in the organic substance concentration in the stripping solution, and can reduce the frequency of analysis and set up operations such as draining, thereby improving work efficiency. In addition, recording on a recording medium such as paper or CDROM makes it easy to create operational instructions and to reference past calculation results.
  • the control means 500 controls the manipulated variables such as the flow rate, pressure, temperature, etc. to the contact tank and the treatment tank within the organic substance concentration management range. Therefore, automatic control is possible based on the difference between the measured organic substance concentration and the calculated organic substance concentration.
  • the flow rate of dissolved organic matter into the contact tank 10 and the discharge flow rate of the stripping solution to the outside of the device can be controlled directly or indirectly by adjusting the manipulated variables such as flow rate, pressure, temperature, etc. .
  • the discharge flow rate of the stripping solution to the outside of the apparatus continuous or periodic discharge of the stripping solution can be mentioned.
  • the inflow rate of organic matter into the contact tank 10 the number of substrates processed per unit time can be increased or decreased.
  • FIG. 4 is a flowchart showing a procedure that the computer executes the organic substance concentration calculation program of this embodiment.
  • the program first causes the computer to execute a process of reading the data stored in the data storage means 100 and the correction coefficient storage means 200 (S30), and then the organic substance concentration The organic substance concentration is calculated by the calculation means 300 (S31), and a signal representing the calculated organic substance concentration is output (S32) —the series of processes is executed.
  • Stripper High purity EC (EC-H) manufactured by Toa Gosei was used as ethylene carbonate.
  • Substrate A glass plate for liquid crystal panels of size 730 x 920mm 2 , aluminum as the gate electrode material is formed by sputtering, and then a cresol novolac resist resin is applied to the film i. ⁇ A substrate that had been developed and then etched and ashed with aluminum was used as the substrate. The resist resin coverage on the substrate is 50%.
  • peeling device and operating conditions As shown in Fig. 5, a circulation type peeling device with two contact tanks was used. The capacity of each tank is 40, 40, 40, 20, 40 L on the river page of the contact tank 10, the contact tank 11, the ozone treatment tank 20, the degassing tank 30, and the regenerated liquid tower 40. Degassing tower 30 power flow to regeneration liquid tower 40 is 20LZmin, resist inflow volume is 0.5mLZ substrate, stripping solution carry-out amount is 13.4mLZ substrate, mist-like stripping solution is carried out by exhaust Is l ⁇ 4LZHr. The stripping solution taken out by the substrate is discharged as waste water after the cleaning process.
  • the mist-like stripping solution in the exhaust can be reduced to lL / Hr by installing a cooling tower (maintained at 40 ° C) above the chamber where the contact treatment is performed.
  • the total amount of stripping liquid in the exhaust and the stripping liquid brought out together with the substrate is the consumption of the stripping liquid.
  • the stripping liquid for consumption is regularly replenished from the new liquid tank 50, and the liquid volume in the stripping device is kept constant.
  • the temperature of the stripping solution in each tank was set to 80 ° C for the contact tank 10 and regenerated liquid tank 40, 60 ° C for the ozone treatment tank 20 and degassing tank 30, and 50 ° C for the new liquid tank 50.
  • Ozone-containing oxygen gas with a concentration of 200 mgZL was introduced into the ozone treatment tank at a flow rate of 15 LZmin by a discharge ozone generator using oxygen gas as a raw material.
  • the substrate processing speed was set to 60 sheets ZHr, and a cooling tower was installed, and the operation was performed with the removal liquid removal amount lLZHr by exhaust. Under this condition, the calculated concentration of resist in the regenerated solution tank 40 (resist concentration calculated assuming that ozone decomposition does not occur) and the actual concentration of resist decomposition products (carboxylic acid and carboxylic acid ester) are , Estimated value after 3 days, 5 days later Z Measured value, 0.0043 / 0.0065, 0. 0103/0. 0152, 0. 0141/0. 021 The correction factor was determined to be 1.51. Note that the unit of organic substance concentration is resist kgZL.
  • the allowable concentration of the resist decomposition product was divided into 0.0216 resist per kgZL.
  • the inside of the peeling device was stopped every 4 days of operation time, and the entire amount of the peeling solution in the device was replaced with a new solution. This liquid exchange operation took 8 hours.
  • the substrate processing speed is 60 sheets ZHr
  • the stripper is operated in a cycle of 4 days of machine operation + 8 hours of liquid replacement
  • the substrate throughput per month is 39,877 sheets
  • Consumption is 2445L, which is 61mL in terms of consumption per substrate.
  • the substrate processing speed was reduced by half to 30 sheets ZHr, and liquid separation was not performed, and stripping was performed by continuous operation.
  • Table 2 shows the results of calculation of resist degradation product concentration under these conditions (correction coefficient is 1.51) and measured values.
  • the equilibrium concentration was 0.00195 kgZL, so it was expected that the allowable concentration would not be exceeded even if the operation time was extended.
  • the force that continued operation of the peeling device until 30 days.
  • Table 2 it can be seen that the organic substance concentration was calculated with high accuracy by comparing the measured resist decomposition product concentration values with the calculated organic concentration values on the 5th, 10th, and 15th working days.
  • the substrate processing amount per month was 21,600
  • the total consumption of liquid stripper liquid per month was 1009L
  • the consumption per substrate was 47mL, which was approximately 24 compared to the test conditions.
  • % Stripping solution was saved. Furthermore, the complicated stripping solution replacement work can be omitted and the number of work steps can be reduced.
  • the substrate processing speed was returned to 60 sheets ZHr, the cooling tower was made shorter than in Example 1, and the amount of exfoliated liquid taken out by exhaust was increased to 1.8 LZHr.
  • Table 3 shows the calculated results and actual measured values of the resist degradation product concentration under these conditions.
  • the calculated equilibrium concentration was 0.0210 kgZL. Therefore, it was expected that the allowable concentration would not be exceeded even if the operation time was extended.
  • the stripping machine continued to run for 30 days, but there was no problem with the stripping performance.
  • Table 3 as in Example 1, comparing the measured resist decomposition product concentration values with the calculated organic material concentration values on the 5th, 10th, and 15th working days, the organic concentration was calculated accurately. I understand that.
  • the substrate processing volume per month is 43,200
  • the total consumption of the liquid stripping solution is 1875L
  • the consumption per substrate is 43mL, which is about 29% peeling compared to the test conditions.
  • the liquid was saved and the production volume was improved by about 7%.
  • the work man-hour associated with the stripping solution replacement work is not necessary.
  • Table 1 below shows the operating conditions and stripping solution consumption described in Comparative Example, Example 1 and Example 2.
  • the organic substance residue derived from the coating material is removed from the substrate from which the coating material has been at least partially peeled by the peeling step using a circulation type peeling device.
  • the circulation type peeling device, the organic matter concentration calculation device, and the organic matter concentration calculation program used in the first embodiment described above are further used by the washing layer 70 and the drying device 80. It is done. That is, in the present embodiment, the contact tank 10, the ozone treatment tank 20, the deaeration tank 30, the regenerative liquid tank 40, the new liquid tank 50, and the contact chamber 60 are used, and a single substrate type continuous substrate processing apparatus is provided. The circulation type peeling device, the washing layer 70, and the drying device 80 are used.
  • FIG. 6 is a schematic view of a circulation type peeling apparatus for explaining the second embodiment of the present invention.
  • the water rinsing tank 70 is a tank that cleans and removes the stripping solution and the resist residue adhering to the substrate after stripping by the stripping solution in the contact chamber 60 with pure water. Then, the stripping solution and the resist residue cleaned and removed from the substrate are processed in a waste water treatment process, which is not shown in the drawings.
  • the drying device 80 is a tank that dries the substrate, which has been washed with pure water in the water washing tank 70, with dry air. Drying is performed by a method such as centrifugal dehydration, hot air, infrared radiation, etc., and the substrate is dried, and the resist residue is also removed by the force on the substrate surface. As a result, the substrate surface is prevented from being contaminated due to the resist residue reattaching to the substrate surface.
  • the resist residue on the substrate is removed by a removing process using the water washing tank 70 and the drying device 80, and then a quality inspection is performed.
  • quality inspection evaluation criteria include the density of resist residue on the substrate.
  • the substrate is a liquid crystal panel
  • the peripheral portion to which the residue is attached is a pixel. Therefore, the probability of black spots or white spots on the liquid crystal panel being displayed increases. Therefore, it is desirable that there is no resist residue on the substrate after the removal step, but in this embodiment, a yield of about 100% is achieved within the required standard range of the liquid crystal panel manufacturer regarding the resist residue.
  • Possible evaluation criteria were adopted as management values.
  • a resist residue density of 1.5 Zm 2 was used as the control value.
  • the productivity of the product substrate (Yield) can be achieved at a level of almost 100%, and if it is within the control value range, the stripping process and removal process can be fully automated.
  • test conditions in the second embodiment are the same as the test conditions in the first embodiment.
  • the substrate processing speed was set to 60 sheets ZHr, and the stripper removal amount by exhaust lLZHr was continuously operated for 30 days. After the peeling process and the removing process, 10 circuit boards are randomly extracted, As a result of observation of the substrate surface with an optical microscope, the resist remaining ⁇ on the substrate surface mean 4. was six Zm 2. The final circuit board yield was 10% or less.
  • the peeling device when the peeling device is operated in a cycle of 4 days of apparatus operation + 8 hours of liquid exchange under the above test conditions where the substrate processing speed is 60 sheets ZHr, The substrate processing amount per unit is 39,877, and the total consumption of stripping solution is 2445L, which is 61mL when converted to the consumption per substrate.
  • the resist remaining ⁇ on the substrate surface mean 2. was one Zm 2.
  • the final circuit board yield was 65%.
  • the peeling process was performed under the same conditions as in Example 2 of the first embodiment described above, and after performing the removal process, 10 circuit boards were randomly extracted, and the substrate surface was observed with an optical microscope. resist residue ⁇ on the substrate surface was averaged 1.0 amino Zm 2. The final circuit board yield was 91%.
  • the coating material is peeled off from the substrate by using the regenerative stripping solution to come into contact with the coating material.
  • the peeling liquid to be filled can be extremely reduced. As a result, it becomes possible to use the stripping solution efficiently, and the consumption of the stripping solution can be greatly reduced, the economy can be improved, and the burden on the environment can be reduced.
  • the concentration change of dissolved organic matter with the operation time after the start of stripping is not calculated based on complicated physical property calculations, but the organic matter is simply and accurately calculated. Concentration can be calculated and changes in organic concentration can be predicted at the same time.
  • the organic substance concentration in the process in the stripping device can be easily managed. As a result, complicated chemical exchange work required for concentration management can be reduced, and stripping solution can be used efficiently. As a result, the consumption of the stripping solution can be greatly reduced, the economy can be improved and the burden on the environment can be reduced.
  • the organic substance concentration in the circulation type peeling apparatus can be calculated easily and accurately, and a change in the organic substance concentration can be predicted. Therefore, since the circulation type peeling apparatus can be operated within the standard of operation control value, contamination of the circuit board, that is, adhesion of resist residue can be avoided. As a result, the yield of circuit boards can be greatly improved.
  • the organic residue on the substrate after the removal step was below a predetermined control value, the number of organic residues on the substrate was adopted as the quality control standard of the substrate as a product. In this case, the product yield can be greatly improved, and continuous production is also possible within the quality control standards.
  • the force exemplified for the peeling apparatus including the ozone treatment mechanism is not limited to the above-described embodiment, and includes various other embodiments.
  • the concentration management becomes easier and the industrial value can be increased.
  • the peeling step since the coating material is peeled off from the substrate by contacting the coating material on the substrate using the regenerative peeling solution, the amount of the newly replenished peeling solution is extremely reduced. be able to. As a result, it becomes possible to use the stripping solution efficiently, and the consumption of the stripping solution can be greatly reduced, the economic efficiency can be improved, and the burden on the environment can be reduced.
  • the coating substance on the substrate is reattached. It is possible to prevent contamination of the substrate surface and improve the product yield due to generation of defective products.
  • the organic residue on the substrate that has been subjected to the removal process is less than or equal to a predetermined control value, if the number of organic residues on the substrate is adopted as the quality control standard of the substrate that is the product, Yield can be greatly improved, and continuous production is also possible within the quality control standards.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • Manufacturing & Machinery (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical & Material Sciences (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)

Abstract

La présente invention concerne un procédé de production d'un substrat qui comprend un stade de décapage, consistant en une étape de traitement d'une solution de décapage qui contient des matières organiques provenant d'un revêtement décapé qui y a été dissous afin d'obtenir une solution de décapage régénérée et en une étape de mise d'une solution de décapage fraîche et de la solution de décapage régénérée au contact d'un revêtement sur un substrat, et un stade d'élimination, consistant en une étape de lavage à l'eau de la surface du substrat d'où le revêtement a été décapé lors du stade de décapage et en une étape de séchage du substrat lavé par un courant d'air de séchage, les matières organiques restant sur le substrat après le stade d'élimination ne dépassant pas un seuil défini.
PCT/JP2006/313234 2005-07-05 2006-07-03 Procédé de production d'un substrat en régulant la concentration en matières organiques dans la solution de décapage WO2007004612A1 (fr)

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EP4306223A1 (fr) * 2021-03-12 2024-01-17 Toray Industries, Inc. Procédé permettant de séparer un revêtement d'un film avec un revêtement, et appareil permettant de séparer un revêtement

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000338684A (ja) * 1999-05-26 2000-12-08 Nagase & Co Ltd 基板表面処理装置
JP2003107755A (ja) * 2001-06-21 2003-04-09 Chi Mei Optoelectronics Corp フォトレジスト剥離液を管理するための方法および装置
JP2003203856A (ja) * 2001-10-23 2003-07-18 Ums:Kk 有機被膜の除去方法
JP2003305418A (ja) * 2002-04-11 2003-10-28 Ums:Kk 基体表面の有機被膜の除去装置
JP2003330206A (ja) * 2001-10-23 2003-11-19 Ums:Kk 有機被膜の除去方法および除去装置
JP2004186389A (ja) * 2002-12-03 2004-07-02 Yokogawa Electric Corp 薬液濃度管理システム
JP2005191030A (ja) * 2003-12-24 2005-07-14 Sharp Corp レジスト除去装置およびレジスト除去方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000338684A (ja) * 1999-05-26 2000-12-08 Nagase & Co Ltd 基板表面処理装置
JP2003107755A (ja) * 2001-06-21 2003-04-09 Chi Mei Optoelectronics Corp フォトレジスト剥離液を管理するための方法および装置
JP2003203856A (ja) * 2001-10-23 2003-07-18 Ums:Kk 有機被膜の除去方法
JP2003330206A (ja) * 2001-10-23 2003-11-19 Ums:Kk 有機被膜の除去方法および除去装置
JP2003305418A (ja) * 2002-04-11 2003-10-28 Ums:Kk 基体表面の有機被膜の除去装置
JP2004186389A (ja) * 2002-12-03 2004-07-02 Yokogawa Electric Corp 薬液濃度管理システム
JP2005191030A (ja) * 2003-12-24 2005-07-14 Sharp Corp レジスト除去装置およびレジスト除去方法

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