JP2000285528A - Production of optical information recording medium - Google Patents

Abstract

PROBLEM TO BE SOLVED: To ensure the reproducibility of recording and reproducing characteristics even when a waste dye solution is reutilized as a dye solution and to efficiently reduce production cost. SOLUTION: In order to wash off a dye which has stuck to the scattering preventing wall 404 of a spin coater during the coating of a substrate with a dye solution by means of the spin coater, the scattering preventing wall 404 is put in a washing tank 602 and washed. At the time when the concentration of the dye in a waste dye solution 604 in the washing tank 602 exceeds that in a waste dye solution 452 recovered in the coating process, these waste dye solutions are mixed to obtain a mixed waste dye solution 606. The dye and a fading inhibitor in the mixed waste dye solution 606 are quantified, the concentrations of the dye and the fading inhibitor in the mixed waste dye solution 606 are made to coincide with those in the dye solution by adjustment with a precision to two or more decimal places and the resulting solution is reutilized as a regenerated dye solution 614.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of manufacturing a heat mode optical information recording medium capable of recording and reproducing information by using a laser beam.

[0002]

2. Description of the Related Art In general, as an optical information recording medium (optical disk) on which information can be recorded only once by a laser beam, there are a write-once CD (so-called CD-R) and a DVD-R. Compared to the production of (compact discs), it has the advantage that a small amount of CDs can be supplied to the market at a reasonable price and quickly, and the demand has increased with the recent spread of personal computers and the like.

A typical structure of a CD-R type optical information recording medium is a recording layer made of an organic dye, a light reflecting layer made of a metal such as gold on a transparent disc-shaped substrate having a thickness of about 1.2 mm,
Further, a protective layer made of resin is laminated in this order (see, for example, JP-A-6-150371).

A DVD-R type optical information recording medium is
It has a structure in which two disc-shaped substrates (having a thickness of about 0.6 mm) are bonded together with their respective information recording surfaces facing inward, and has a feature that the amount of recorded information is large.

For writing (recording) information on these optical information recording media, a laser beam in the near-infrared region (a laser beam having a wavelength of about 780 nm for CD-R and a wavelength of about 635 nm for DVD-R) is irradiated. The irradiation portion of the dye recording layer absorbs the light and locally raises the temperature, causing a physical or chemical change (for example, formation of pits) and changing its optical characteristics. Information is recorded.

On the other hand, information reading (reproduction) is usually
Reflection is performed by irradiating a laser beam having the same wavelength as the recording laser beam, so that the optical characteristics of the dye recording layer are changed between a portion (recorded portion due to pit generation) and a portion not changed (unrecorded portion). The information is reproduced by detecting the difference in rate.

[0007]

By the way, a spin coating method is used for manufacturing the above-mentioned optical disk. In this spin coating method, a solution is dropped on the inner peripheral side of a rotating substrate, and the solution is cast on the outer peripheral side by centrifugal force to form a coating film. This is a type of thin film forming method including a process of shaking off from a part, discharging the solution around the part, and then drying and removing the solvent from the coating film.

In order to provide an optical disk at low cost, it is important to manufacture the optical disk at a low cost. To do so, (1) use inexpensive raw materials. (2) To increase the production yield. (3) To increase production speed. Becomes important.

[0009] Among them, with regard to (1), it is difficult to reduce the price of the raw materials further, and it is necessary to consider a new method.

Therefore, as a method to be noticed, there is a method of reusing a waste liquid discharged in a coating treatment by a spin coating method. That is, the amount actually applied on the substrate by the spin coating method is about 20% of the discharge amount, and the rest is accumulated in the waste liquid reservoir. If this can be reused, manufacturing costs can be significantly reduced.

The present invention has been made in view of such problems, and can ensure reproducibility of recording / reproducing characteristics even when a dye waste liquid is reused as a dye solution, thereby efficiently realizing reduction in manufacturing cost. It is an object of the present invention to provide a method for manufacturing an optical information recording medium that can be made to operate.

Another object of the present invention is to provide a method of manufacturing an optical information recording medium capable of improving the recovery rate of a dye waste liquid and improving production efficiency in addition to the above-mentioned conditions. It is in.

[0013]

According to the present invention, there is provided a method of manufacturing a heat mode type optical information recording medium having a dye recording layer on which information can be recorded by irradiating a laser beam on the substrate. A coating step of applying a dye solution for forming the dye recording layer on the substrate while rotating, a collection step of collecting a dye waste liquid discharged in the coating step, and a surrounding area when coating the dye solution. A washing step of washing the dye adhering to the substrate, and mixing of these dye waste liquids at a stage where the dye concentration of the dye waste liquid collected in the washing step is equal to or higher than the dye concentration of the dye solution collected in the collection step. And a mixing step, wherein the mixed dye waste liquid obtained in the mixing step is reused as a dye solution.

That is, the dye waste liquid collected in the washing step and the dye waste liquid discharged in the coating treatment of the dye solution (the dye waste liquid collected in the recovery step) are mixed to form a mixed dye waste liquid.
Since this mixed dye waste liquid is reused as a dye solution, the recovery rate of the dye waste liquid can be greatly increased, and the production efficiency can be improved.

In particular, when the dye concentration of the dye waste liquid recovered in the washing step becomes higher than the dye concentration of the dye solution recovered in the recovery step, these dye waste liquids are mixed. It is possible to prevent impurities from entering the inside, to ensure reproducibility of recording / reproducing characteristics even if the mixed dye waste liquid is reused as a dye solution, and to efficiently realize a reduction in manufacturing cost.

The cleaning step may include a process of cleaning an apparatus for applying a dye solution onto the substrate using a cleaning tank. In this case, immersion washing is preferable. By immersing the dye adhering to the apparatus in the washing tank for washing, the dye waste liquid accumulates in the washing tank, and the dye waste liquid can be obtained efficiently. The time for immersing the dye in the washing tank is preferably 10 minutes or more, preferably 30 minutes.
A minute or more is good.

In the above-mentioned manufacturing method, when the dye solution contains a dye and an anti-fading agent, a step of quantifying the content of the dye and the anti-fading agent in the mixed dye waste liquid; Adjusting the concentrations of the dye and the anti-fading agent in the dye solution so as to match the concentrations of the dye and the anti-fading agent with two or more digits of accuracy. Thereby, even when the mixed dye waste liquid is reused as the dye solution, reproducibility of the recording / reproducing characteristics can be ensured.

In this case, it is preferable that the amount of the dye and the anti-fading agent in the mixed dye waste liquid is determined by liquid chromatography.
It is preferably more than an order of magnitude.

Further, it is preferable to store the mixed dye waste liquid in a closed container which does not transmit light. In this case, the degree of cleanliness during storage of the mixed dye waste liquid may be set to 500,000 or less, preferably 200,000 or less.

In the case where an edge cleaning step of removing a portion corresponding to the outer peripheral edge of the substrate from the coating solution of the dye solution formed on the substrate is included, the waste liquid at the time of edge cleaning is replaced with the dye waste liquid. Separation is preferred.

In the case where the method includes a back surface cleaning step of removing a coating film adhered to the back surface of the substrate among the coating films of the dye solution formed on the substrate, the waste liquid from the back surface cleaning may be replaced with the dye waste liquid. It is preferable to separate them.

Separation of the waste liquid at the time of edge cleaning and the waste liquid at the time of back surface washing from the dye waste liquid can prevent impurities from being mixed in the process. Even when the mixed dye waste liquid is reused as the dye solution, recording and reproduction can be performed. Reproducibility of characteristics can be secured.

The exhaust air velocity at the time of applying the dye solution is 1 m / s or less, preferably 0.7 m / s or less, and more preferably 0.4 m / s or less. Thus, the dye solution can be favorably applied to the substrate, and the recovery rate of the dye waste liquid can be improved.

When a dye solution is applied on the substrate to form the dye recording layer, the discharge amount of the dye solution is set to 0.3.
It is preferably between cc and 5 cc, more preferably between 0.5 cc and 2 cc.

The temperature at which the dye solution is applied is 10 ° C.
To 50 ° C, preferably 15 ° C to 35 ° C.
C, more preferably in the range of 20 to 25C.

The humidity at the time of applying the dye solution is 25%
The range of RH to 65% RH is suitable, preferably 35%.
% RH to 60% RH, more preferably 45% RH
It is in the range of ５５55% RH.

[0027]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, an embodiment in which a method for manufacturing an optical information recording medium according to the present invention is applied to a system for manufacturing an optical disk such as a CD-R (hereinafter simply referred to as a manufacturing system according to the embodiment). Will be described with reference to FIGS.

The manufacturing system 10 according to the present embodiment
As shown in FIG. 1, for example, two molding equipments (first and second molding apparatuses) for producing a substrate by injection molding, compression molding or injection compression molding.
And a second molding facility 12A and 12B), a coating facility 14 for forming a dye recording layer on the substrate by applying and drying a dye coating solution on one main surface of the substrate, and a dye recording apparatus for the substrate. A light-reflecting layer is formed on the light-reflecting layer by, for example, sputtering, and after that, a UV curing liquid is applied onto the light-reflecting layer, and then UV irradiation is performed to form a protective layer on the light-reflecting layer. It is configured.

First and second molding equipment 12A and 12B
Is a molding machine 20 for injection molding, compression molding, or injection compression molding of a resin material such as polycarbonate to produce a substrate having a tracking groove or an unevenness (groove) representing information such as an address signal formed on one main surface. A cooling unit 22 for cooling the substrate taken out of the molding machine 20, and an accumulating unit 26 (stack pole turntable) on which a plurality of stack poles 24 for stacking and storing the cooled substrates are stored.
And

The coating equipment 14 has three processing units 30, 32
And 34, the first processing section 30 includes a stack pole storage section 40 for storing the stack poles 24 transported from the first and second molding facilities 12A and 12B, and a stack pole storage section 40 for storing the stack poles. A first transport mechanism 42 that takes out the substrates one by one from the stack pole 24 accommodated in the unit 40 and transports the substrates to the next process; And an electrostatic blow mechanism 44 for removing.

The second processing section 32 includes a second transport mechanism 46 for sequentially transporting the substrates, which have been subjected to the electrostatic blow processing in the first processing section 30, to the next step, and transporting the substrates by the second transport mechanism 46. A dye coating mechanism 48 that applies a dye coating liquid to each of the plurality of substrates, and a third transport mechanism 50 that transports the substrates that have been subjected to the dye application processing one by one to the next process. The dye application mechanism 48 includes six spin coaters 52.

The third processing section 34 cleans the back surface of one substrate transported by the third transport mechanism 50, and transports the substrate after the back surface cleaning to the next step. A fourth transport mechanism 56, a numbering mechanism 58 for marking the substrate transported by the fourth transport mechanism 56 with a lot number or the like, and transporting the substrate having been stamped with the lot number or the like to the next step. A fifth transport mechanism 60, an inspection mechanism 62 that inspects the substrate transported by the fifth transport mechanism 60 for the presence or absence of a defect, and a film thickness of the dye recording layer, and an inspection by the inspection mechanism 62. Depending on the result, the substrate is replaced with a stack pole 64 for normal products or a stack pole 66 for NG.
And a sorting mechanism 68 for sorting the pieces.

A first partition plate 70 is provided between the first processing unit 30 and the second processing unit 32, and the second processing unit 32 and the third processing unit 34 have the same second processing unit. A partition plate 72 is provided. An opening (not shown) is formed below the first partition plate 70 to such an extent that the transfer path of the substrate by the second transfer mechanism 46 is not blocked. An opening (not shown) is formed so as not to block the substrate transfer path by the third transfer mechanism 50.

The post-processing facility 16 includes a stack pole storage section 80 for storing a stack pole 64 for normal products transported from the coating apparatus 14, and one of the stack poles 64 stored in the stack pole storage section 80. A sixth transport mechanism 82 that takes out substrates one by one and transports them to the next process;
A first electrostatic blow mechanism 84 for removing static electricity from one substrate transported by the sixth transport mechanism 82
And a seventh transport mechanism 86 for sequentially transporting the substrate after the electrostatic blow processing to the next step, and forming a light reflecting layer on one main surface of the substrate transported by the seventh transport mechanism 86 by sputtering. Transport mechanism 90 for sequentially transporting the substrate after the sputtering of the light reflection layer to the next step, and cleaning the periphery (edge portion) of the substrate transported by the eighth transport mechanism 90 Edge cleaning mechanism 9
And 2.

Further, the post-processing equipment 16 includes a second electrostatic blow mechanism 94 for removing static electricity from the substrate after edge cleaning, and a second electrostatic blow mechanism 94 for removing one main surface of the substrate after electrostatic blow processing. UV curable liquid application mechanism 96 for applying UV curable liquid
And a spin mechanism 9 for rotating the substrate on which the UV curing liquid has been applied at a high speed so as to make the applied thickness of the UV curing liquid on the substrate uniform.
8, a UV irradiation mechanism 10 for curing the UV curing liquid by irradiating ultraviolet rays to the substrate after the application of the UV curing liquid and the spin treatment to form a protective layer on one main surface of the substrate
0 and a second electrostatic blow mechanism 94, a UV curing liquid coating mechanism 96, a spin mechanism 98 and a UV irradiation mechanism 10
And a tenth transport mechanism 10 for transporting the substrate irradiated with UV to the next step.
4, a defect inspection mechanism 106 for inspecting the substrate transported by the tenth transport mechanism 104 for defects on the coating surface and the protective layer surface, and a defect inspection mechanism 106 for inspecting signal characteristics due to grooves formed on the substrate. It has a characteristic inspection mechanism 108 and a selection mechanism 114 for selecting a substrate into a stack pole 110 for a normal product or a stack pole 112 for NG according to the inspection results of the defect inspection mechanism 106 and the characteristic inspection mechanism 108.

Here, the configuration of one spin coater 52 will be described with reference to FIGS.

As shown in FIGS. 2 and 3, the spin coater 52 includes a coating liquid applying device 400, a spinner head device 402, and a scattering prevention wall 404. The coating liquid application device 400 includes a pressurized tank (not shown) filled with the coating liquid, and a nozzle 40 from the pressurized tank.
6, a pipe (not shown) and a nozzle 406
And a discharge amount adjustment valve 408 for adjusting the amount of the coating liquid discharged from the substrate 202. A predetermined amount of the coating liquid is dropped on the surface of the substrate 202 through the nozzle 406. The coating liquid application device 400 includes a nozzle 4
Support plate 410 supporting supporter 06 downward and support plate 4
A handling mechanism 414 having a motor 412 for horizontally rotating the substrate 10 causes the substrate 20 to move from the standby position.
2 so as to be able to turn to a position above.

The spinner head device 402 is disposed below the coating liquid application device 400, holds the substrate 202 horizontally by a detachable fixing tool 420, and rotates the substrate 202 by a drive motor (not shown). It is possible to rotate.

The coating liquid dropped from the nozzle 406 of the coating liquid applying device 400 onto the substrate 202 rotating while being held horizontally by the spinner head device 402 is directed outward on the surface of the substrate 202. Cast. And
The excess coating liquid is shaken off at the outer peripheral edge of the substrate 202, discharged to the outside, and then dried to form a coating film (dye recording layer 204) on the surface of the substrate 202.

The scattering prevention wall 404 is provided to prevent the excess coating solution discharged outward from the outer peripheral edge of the substrate 202 from scattering to the periphery, and has an opening 422 at the top.
Are formed around the spinner head device 402 so as to be formed. The excess coating liquid collected through the scattering prevention wall 404, that is, the dye waste liquid, is collected in the collection container 450 through the drain 424. The processing after the collection of the dye waste liquid will be described later in detail.

The local exhaust of each of the spin coaters 52 in the second processing unit 32 (see FIG. 1) causes air taken in from the opening 422 formed above the scattering prevention wall 404 on the surface of the substrate 202. Exhaust pipe 42 attached below each spinner head device 402.
6 to be exhausted. The exhaust wind speed at this time is set to 1 m / s or less.

The nozzle 406 of the coating liquid application device 400
As shown in FIGS. 4 and 5, an elongated cylindrical nozzle main body 432 having a through hole 430 formed in the axial direction, and a mounting portion 434 for fixing the nozzle main body 432 to the support plate 410 (see FIG. 3). Having. The nozzle body 432 has a front end surface and a surface whose outside or inside, or both wall surfaces within 1 mm or more from the front end surface, are made of a fluorine compound. As the fluorine compound, for example, polytetrafluoroethylene, a substance containing polytetrafluoroethylene, or the like can be used.

As an example of a preferred nozzle 406 used in this embodiment, for example, as shown in FIG. 5, a tip surface of a nozzle body 432 and a range of 1 mm or more from the tip surface are formed using a fluorine compound. Nozzle 406
Alternatively, as shown in FIG.
Nozzles 406 whose outer and / or inner surfaces within a range of 1 mm or more from 0 and the tip surface 440 thereof, or both wall surfaces 442 and 444 are coated with a fluorine compound.

When the tip surface of the nozzle body 432 and the area of 1 mm or more from the tip surface are formed of a fluorine compound,
In consideration of the strength and the like, it is practically preferable that the nozzle body 432 is formed of, for example, stainless steel, and that the front end face and the range of up to 5 mm from the front end face are formed of a fluorine compound.

Further, as shown in FIG.
In the case where the front end surface 440 and the outer or inner side of the end surface 440 or more or 1 mm or more, or both of the wall surfaces 442 and 444 are coated with a fluorine compound, the nozzle body 43
10 mm or more from the tip surface 440 of the second, more preferably,
Preferably, the entire area of the nozzle body 432 is covered with a fluorine compound. The thickness of the coating is not particularly limited, but is suitably in the range of 5 to 500 μm. As described above, stainless steel is preferable as the material of the nozzle body 432. The diameter of the through hole 430 formed in the nozzle main body 432 is generally in the range of 0.5 to 1.0 mm.

Next, a process of manufacturing the optical disc D by the manufacturing system 10 will be described with reference to the process charts of FIGS. 7A to 8B.

First, in a molding machine 20 in each of the first and second molding facilities 12A and 12B, a resin material such as polycarbonate is subjected to injection molding, compression molding or injection compression molding, and as shown in FIG. A groove 2 for representing information such as a tracking groove or an address signal;
The substrate 202 on which the “00” is formed is manufactured.

Examples of the material of the substrate 202 include acrylic resins such as polycarbonate and polymetal methacrylate, vinyl chloride resins such as polyvinyl chloride and vinyl chloride copolymer, epoxy resins, amorphous polyolefin and polyester. They can be used together if desired. Among the above materials, polycarbonate is preferred from the viewpoints of moisture resistance, dimensional stability, cost, and the like. The depth of the groove 200 is 0.0
It is preferably in the range of 1 to 0.3 μm, and its half width is preferably in the range of 0.2 to 0.9 μm.

The substrate 202 taken out of the molding machine 20
After being cooled in the cooling unit 22 in the subsequent stage, the wafer is stacked on the stack pole 24 with one main surface directed downward. At the stage when a predetermined number of substrates 202 are stacked on the stack pole 24, the stack pole 24 is taken out from the molding facilities 12A and 12B, and is conveyed to the next coating facility 14, where the stack pole storage section 40 in the coating facility 14 is placed.
To be housed. This transfer may be performed by a trolley or by a self-propelled automatic transfer device.

At the stage when the stack pole 24 is housed in the stack pole housing section 40, the first transport mechanism 42 operates, and the substrates 202 are taken out one by one from the stack pole 24 and sent to the subsequent electrostatic blow mechanism 44. Transport. After the static electricity is removed by the electrostatic blow mechanism 44, the substrate 202 transported to the electrostatic blow mechanism 44 is transported to the next dye coating mechanism 48 via the second transport mechanism 46, and is subjected to six spin coatings. One of the devices 52 is supplied to one of the spin coaters 52. The substrate 202 loaded into the spin coater 52 is applied with a dye coating solution on one main surface thereof, is rotated at high speed to make the thickness of the coating solution uniform, and then subjected to a drying process. As a result, FIG.
As shown in FIG. 2, the dye recording layer 20 is formed on one main surface of the substrate 202.
4 will be formed.

That is, the substrate 202 loaded in the spin coater 52 is mounted on a spinner head device 402 shown in FIG. Next, a predetermined amount of the application liquid supplied from the pressurized tank is adjusted by the discharge amount adjustment valve 408, and the applied liquid is dropped on the inner peripheral side of the substrate 202 through the nozzle 406.

As described above, since the nozzle 406 has a front end surface and an outer or inner surface within 1 mm or more from the front end surface, or both of the wall surfaces, the surface is made of a fluorine compound. Adhesion does not easily occur, and it is hard to dry to cause precipitation of the dye and its deposit. Therefore, the coating film can be formed smoothly without obstruction such as coating film defects.

As the coating solution, a dye solution in which a dye is dissolved in an appropriate solvent is used. The concentration of the dye in the coating solution is generally in the range of 0.01 to 15% by weight, preferably in the range of 0.1 to 10% by weight, particularly preferably 0.5 to 10% by weight.
It is in the range of 5% by weight, most preferably in the range of 0.5-3% by weight.

The spinner head device 402 can be rotated at a high speed by a drive motor. The coating solution dropped on the substrate 202 is rotated by the rotation of the spinner head device 402.
It is cast on the surface of the substrate 202 in the outer peripheral direction, and reaches the outer peripheral edge of the substrate 202 while forming a coating film. The excess coating solution that has reached the outer peripheral edge is further shaken off by centrifugal force and scattered around the edge of the substrate 202. The excess application liquid that has scattered collides with the scatter prevention wall 404, is collected in a tray provided below the scatter prevention wall 404, and is collected through the drain 424. Drying of the coating film is performed during the formation process and after the formation of the coating film. The thickness of the coating film (dye recording layer 204) is generally 2
0-500 nm, preferably 50-300 nm.
nm.

The dye used in the dye recording layer 204 is not particularly limited. Examples of usable dyes include cyanine dyes, phthalocyanine dyes, imidazoquinoxaline dyes, pyrylium / thiopyrylium dyes, azurenium dyes, squalilium dyes, metal complex salt dyes such as Ni and Cr, and naphthoquinone dyes And anthraquinone dyes, indophenol dyes, indoaniline dyes, triphenylmethane dyes, merocyanine dyes, oxonol dyes, aminium / diimmonium dyes, and nitroso compounds. Among these dyes, cyanine dyes are preferable, benzoindolenine dyes are more preferable, and dyes represented by the following general formula (1) are particularly preferable.

[0056]

Embedded image

R ^{1 in the} general formula (1) represents a monovalent substituent. As the monovalent substituent, a substituted or unsubstituted alkyl group is preferable. The alkyl group is preferably an alkyl group having 1 to 18 carbon atoms, more preferably an alkyl group having 1 to 12 carbon atoms, and particularly preferably an alkyl group having 1 to 4 carbon atoms.

The alkyl group may be linear or branched. Examples of the substituent include a halogen atom such as a fluorine atom and a chlorine atom; an alkoxy group such as a methoxy group and an ethoxy group; an alkylthio group such as a methylthio group and a methylthio group; Acyl groups such as acetyl groups; hydroxy groups; alkoxycarbonyl groups such as ethoxycarbonyl groups; alkenyl groups such as vinyl groups; and aryl groups such as phenyl groups.

R of the general formula (1)^TwoAnd R^ThreeRespectively
And independently represents a monovalent substituent. As the monovalent substituent,
A substituted or unsubstituted alkyl group is preferred. The alkyl group is
An alkyl group having 1 to 4 carbon atoms is preferable, a methyl group,
Ethyl groups are particularly preferred. R ^TwoAnd R^ThreeIs connected to each other
To form a ring.

R ^{4 in the} general formula (1) represents a monovalent substituent. Examples of the monovalent substituent include a hydrogen atom, a carbon atom having 1 to 16 carbon atoms.
Are preferably an alkyl group, a halogen atom and an aralkyl group, more preferably a methyl group, an ethyl group and a benzyl group, and particularly preferably a methyl group.

X ^{n- in the} general formula (1) represents an anion;
n represents 1, 2 or 3. As anions, halide ions, sulfonate ions, ClO ₄ ⁻ , BF ₄ ⁻ ,
SbF ₅ ⁻ , metal complex ions and phosphate ions can be mentioned. Among these, a divalent anion (n = 2) is preferable, and a divalent anion represented by the following general formula (2) is particularly preferable.

[0062]

Embedded image

R ^{5 to} R ¹⁰ in the general formula (2) each independently represent a monovalent substituent. As the monovalent substituent, a hydrogen atom, an alkyl group, a halogen atom and an aralkyl group are preferable, a hydrogen atom and an alkyl group having 8 or less carbon atoms are more preferable, and a methyl group is particularly preferable.

Examples of the solvent of the coating agent for forming the dye recording layer 204 include esters such as butyl acetate and cellosolve acetate; ketones such as methyl ethyl ketone, cyclohexanone and methyl isobutyl ketone; dichloromethane, 1,2-dichloroethane, chloroform. Chlorinated hydrocarbons such as amides; amides such as dimethylformamide;
Hydrocarbons such as cyclohexane; tetrahydrofuran,
Ethers such as ethyl ether and dioxane; alcohols such as ethanol, n-propanol, isopropanol, n-butanol and diacetone alcohol;
Fluorinated solvents such as 2,3,3-tetrafluoro-1-propanol; ethylene glycol monomethyl ether;
Examples thereof include glycol ethers such as ethylene glycol monoethyl ether and propylene glycol monomethyl ether.

The above-mentioned solvents may be used alone or in combination of two or more kinds in consideration of the solubility of the dye used. Preferably, it is a fluorinated solvent such as 2,2,3,3-tetrafluoro-1-propanol. In the coating solution, an anti-fading agent or a binder may be added as desired, or various additives such as an antioxidant, a UV absorber, a plasticizer, and a lubricant may be added according to the purpose. It may be added.

Representative examples of the anti-fading agent include nitroso compounds, metal complexes, diimmonium salts and aminium salts. These examples are described in, for example, JP-A-2-300288, JP-A-3-224793, and JP-A-4-224793.
No. 146189.

In this embodiment, an anti-fading agent represented by the following general formula (3) is preferred.

[0068]

Embedded image

R ¹¹ and R ^{12 in} formula (3) each represent an independent hydrogen atom or a monovalent substituent.

The substituents represented by R ¹¹ and R ¹² are a halogen atom or a substituent obtained by combining a carbon atom, an oxygen atom, a nitrogen atom or a sulfur atom, and specifically include an alkyl group, an alkenyl group, Aralkyl, aryl, heterocyclic, halogen, cyano, nitro, mercapto, hydroxy, alkoxy, aryloxy, alkylthio, arylthio, acyloxy, amino, alkylamino, amide groups , Sulfonamide group, sulfamoylamino group, alkoxycarbonylamino group, alkoxysulfonylamino group, ureido group, thioureido group, acyl group, alkoxycarbonyl group, carbamoyl group, alkylsulfonyl group, alkylsulfinyl group, sulfamoyl group, carboxyl group (Including salt), sul There can be mentioned groups (including salts). These may be further substituted with these substituents.

R ¹¹ and R ¹² each independently represent a hydrogen atom,
An alkyl group having 1 to 6 carbon atoms, a halogen atom, a cyano group,
An alkoxy group having 1 to 6 carbon atoms, an alkylthio group having 1 to 6 carbon atoms, an amide group having 1 to 6 carbon atoms, a sulfonamide group having 1 to 6 carbon atoms, a ureido group having 1 to 6 carbon atoms,
Preferred are an acyl group having 6 carbon atoms, an alkoxycarbonyl group having 2 to 6 carbon atoms, a carbamoyl group having 1 to 6 carbon atoms, an alkylsulfonyl group having 1 to 6 carbon atoms, and an alkylsulfinyl group having 1 to 6 carbon atoms. The following alkoxy groups are more preferable, and methoxy groups and ethoxy groups are particularly preferable.

Examples of the binder include natural organic high molecular substances such as gelatin, cellulose derivatives, dextran, rosin, and rubber; and hydrocarbon resins such as polyethylene, polypropylene, polystyrene, and polyisobutylene; polyvinyl chloride; Vinylidene, polyvinyl chloride
Vinyl resins such as polyvinyl acetate copolymer, acrylic resins such as polymethyl acrylate and polymethyl methacrylate, polyvinyl alcohol, chlorinated polyethylene, epoxy resin, butyral resin, rubber derivatives, phenol
Synthetic organic polymers such as precondensates of thermosetting resins such as formaldehyde resins can be mentioned.

When a binder is used, the amount of the binder used is generally 20 parts by weight or less, preferably 10 parts by weight or less, more preferably 5 parts by weight, based on 100 parts by weight of the dye.
Not more than parts by weight.

The thickness of the dye recording layer 204 is generally 20 to
It is provided in the range of 500 nm, preferably in the range of 50 to 300 nm.

Incidentally, an undercoat layer may be provided on the substrate surface on the side where the dye recording layer 202 is provided, for the purpose of improving flatness, improving adhesive strength, preventing deterioration of the dye recording layer 204, and the like. .

Examples of the material for the undercoat layer include polymethyl methacrylate, acrylic acid / methacrylic acid copolymer,
Styrene / maleic anhydride copolymer, polyvinyl alcohol, N-methylol acrylamide, styrene / vinyl toluene copolymer, chlorosulfonated polyethylene,
Nitrocellulose, polyvinyl chloride, chlorinated polyolefin, polyester, polyimide, vinyl acetate-vinyl chloride copolymer, ethylene-vinyl acetate copolymer, polyethylene, polypropylene, polycarbonate and other high-molecular substances, and silane coupling agents Surface modifiers can be mentioned.

The undercoat layer is prepared by dissolving or dispersing the above substance in an appropriate solvent to prepare a coating solution, and then applying the coating solution to the substrate surface by using a coating method such as spin coating, dip coating, or extrusion coating. Can be formed. The thickness of the undercoat layer is generally 0.005.
It is provided in the range of ２０20 μm, preferably in the range of 0.01 to 10 μm.

The substrate 202 on which the dye recording layer 204 is formed
Is transferred to the next back surface cleaning mechanism 54 via the third transport mechanism 50.
And the other side of the main surface of the substrate 202 (back side)
Is washed. Thereafter, the substrate 202 is transported to the next numbering mechanism 58 via the fourth transport mechanism 56, and the substrate 2
02 is engraved with a lot number or the like on one main surface or the back surface.

Thereafter, the substrate 202 is moved to the fifth transport mechanism 6
Then, the substrate 202 is transported to the next inspection mechanism 62 through which the presence or absence of a defect in the substrate 202 and the thickness of the dye recording layer 204 are inspected. This inspection is performed by irradiating light from the back surface of the substrate 202 and performing image processing on the transmission state of the light using, for example, a CCD camera. The inspection result of the inspection mechanism 62 is sent to the next sorting mechanism 68.

The substrate 202 that has been subjected to the above-described inspection processing is transported and sorted by the sorting mechanism 68 into a stack pole 64 for normal products or a stack pole 66 for NG based on the inspection result.

At the stage when a predetermined number of substrates 202 are loaded on the stack pole 64 for normal products, the stack pole 64 for normal products is taken out of the coating equipment 14 and transported to the next post-processing equipment 16. It is housed in the stack pole housing section 80 of the post-processing facility 16. This transfer may be performed by a trolley or by a self-propelled automatic transfer device.

At the stage when the stack poles 64 for normal products are accommodated in the stack pole accommodating section 80, the sixth transport mechanism 82 operates, and the substrates 2 are stacked one by one from the stack poles 64.
02 is taken out and transported to the first electrostatic blow mechanism 84 at the subsequent stage. After the static electricity is removed by the first electrostatic blow mechanism 84, the substrate 202 transported to the first electrostatic blow mechanism 84 is transported to the next sputtering mechanism 88 via the seventh transport mechanism 86. You. As shown in FIG. 7C, the light reflecting layer 208 is formed on the entire surface of one main surface of the substrate 202 excluding the peripheral portion (edge portion) 206 by sputtering.

The light-reflective substance, which is the material of the light-reflective layer 208, is a substance having a high reflectance with respect to laser light, such as Mg, Se, Y, Ti, Zr, Hf, V, and N.
b, Ta, Cr, Mo, W, Mn, Re, Fe, Co,
Ni, Ru, Rh, Pd, Ir, Pt, Cu, Ag, A
u, Zn, Cd, Al, Ga, In, Si, Ge, T
e, Pb, Po, Sn, Bi, and other metals and semi-metals or stainless steel.

Among these, preferred are Cr, N
i, Pt, Cu, Ag, Au, Al and stainless steel. These substances may be used alone or in combination of two or more. Alternatively, it may be used as an alloy. Particularly preferred is Ag or an alloy thereof.

The light reflecting layer 208 can be formed on the recording layer by, for example, vapor deposition, sputtering or ion plating of the light reflecting substance.
The thickness of the reflective layer is generally in the range of 10 to 800 nm,
Preferably in the range of 20 to 500 nm, more preferably 5
It is provided in the range of 0 to 300 nm.

The substrate 202 on which the light reflecting layer 208 is formed
Is transferred to the next edge cleaning mechanism 9 via the eighth transport mechanism 90.
8A, and as shown in FIG. 8A, the edge portion 206 in one main surface of the substrate 202 is cleaned, and
The dye recording layer 204 formed at 06 is removed.
Thereafter, the substrate 202 is transported to the next second electrostatic blow mechanism 94 via the ninth transport mechanism 102, and the static electricity is removed.

After that, the substrate 202 is transported to the UV curing liquid application mechanism 96 via the ninth transport mechanism 102 as well, and the UV curing liquid is dropped on a part of one main surface of the substrate 202. Thereafter, the substrate 202 is also transported to the next spin mechanism 98 via the ninth transport mechanism 102 and rotated at a high speed, so that the applied thickness of the UV curing liquid dropped on the substrate 202 is reduced over the entire surface of the substrate. Is made uniform.

In this embodiment, time management is performed so that the time from the formation of the light reflection layer to the application of the UV curing liquid is 2 seconds or more and 5 minutes or less.

Thereafter, the substrate 202 is transported to the next UV irradiation mechanism 100 via the ninth transport mechanism 102, and the UV curing liquid on the substrate 202 is irradiated with ultraviolet rays. As a result, as shown in FIG.
An optical disk D is formed by forming a protective layer 210 of a UV curable resin so as to cover the dye recording layer 204 and the light reflecting layer 208 formed on one main surface of the optical disk D.

The protective layer 210 includes the dye recording layer 204 and the like.
On the light reflection layer 208 for physical and chemical protection
Provided. The protective layer 210 is a dye recording layer of the substrate 202
Increases scratch resistance and moisture resistance even on the side where 204 is not provided
It can also be provided for the purpose. Used in the protective layer 210
As the material, for example, SiO, SiO_Two, Mg
F _Two, SnO_Two, Si_ThreeN_FourAnd other inorganic substances, and thermoplastics
Organic such as thermosetting resin, thermosetting resin, and UV curable resin
Substances can be mentioned.

The protective layer 210 can be formed, for example, by laminating a film obtained by extrusion of plastic onto the light reflecting layer 208 and / or the substrate 202 via an adhesive. Alternatively, it may be provided by a method such as vacuum deposition, sputtering, or coating.
In the case of a thermoplastic resin or a thermosetting resin, they can also be formed by dissolving these in an appropriate solvent to prepare a coating solution, applying the coating solution, and drying.

In the case of a UV-curable resin, as described above, a coating solution is prepared as it is or dissolved in an appropriate solvent, and then the coating solution is applied, and the coating solution is irradiated with UV light to be cured. can do. Various additives such as an antistatic agent, an antioxidant, and a UV absorber may be added to these coating solutions according to the purpose. The thickness of the protective layer 210 is generally provided in the range of 0.1 to 100 μm.

Thereafter, the optical disk D is transported to the next defect inspection mechanism 106 and characteristic inspection mechanism 108 via the tenth transport mechanism 104, where the surface of the dye recording layer 204 and the protective layer 2
10, the presence or absence of a defect on the surface of the optical disc D
The signal characteristics of the groove 200 formed in the second groove 2 are inspected. These inspections are performed by irradiating light to both sides of the optical disc D and subjecting the reflected light to image processing by, for example, a CCD camera. The inspection results of the defect inspection mechanism 106 and the characteristic inspection mechanism 108 are sent to the next selection mechanism 114.

The optical disc D, which has been subjected to the above-described defect inspection processing and characteristic inspection processing, has a sorting mechanism 1 based on each inspection result.
Depending on 14, stack pole 110 for normal product or NG
Is sorted by the stack pole 112 for use.

When a predetermined number of optical discs D are loaded on the stack pole 110 for normal products, the stack pole 110 is taken out of the post-processing equipment 16 and put into a label printing step (not shown).

Further, the manufacturing system 1 according to the present embodiment
0, the air conditioning system 300 is installed in parallel with the second processing unit 32 of the coating equipment 14 as shown in FIG. 1, and the first processing unit 30 Air conditioners 704 and 706 are installed on each ceiling of the third processing unit 34 via high-performance packed bed filters (HEPA filters) 700 and 702, respectively.

The air conditioners 704 and 706 include the first and third air conditioners.
By sending clean air to the first and third processing units 30 and 34, respectively.
The temperature inside can be controlled.

As shown in FIGS. 9 and 14, an air conditioning system 300 provided in parallel with the coating equipment 14 takes in an air conditioner 302 for sending clean air ca to the coating equipment 14 and an outside air ea. And a dehumidifier 304 for performing dehumidification and outputting as primary air a1, and an exhaust device 306 (see FIG. 12) for sending some exhaust (local exhaust) da from the coating equipment 14 to an upper exhaust system. It is configured. As the local exhaust da, for example, the coating equipment 14
Spin coaters 5 in the dye coating mechanism 48
2 exhaust.

On the other hand, as shown in FIGS. 9 and 10, the air conditioning system 300 comprises a dehumidifier 304 and an air conditioner 30.
2 and the primary air a1 output from the dehumidifier 304
A duct 310 for sending the air to the air conditioner 302 is provided. As shown in FIG. 12, between each exhaust side of the six spin coaters 52 and the exhaust device 306 in the dye coating mechanism 48 of the coating equipment 14. The exhaust pipe 426 described above
Is provided.

A plurality (four in the illustrated example) between the air conditioner 302 and the coating equipment 14 for supplying the clean air ca output from the air conditioner 302 to the coating equipment 14. Air supply ducts 320a to 320d and coating equipment 1
4 to return the exhaust ra other than the local exhaust da to the air conditioner 302 (8 in the illustrated example).
Book return duct 322 is installed.

[0101] The air conditioner 302 is provided with an inlet 710 for taking in the outside air ea.
A pre-filter 712 is attached to 10. In normal air-conditioning control (when the low-humidity control is not performed), the air taken in from the inlet 710 is supplied to the air conditioner 302 as primary air.

The dehumidifier 304 is used for low humidity control. As shown in FIGS. 9 and 10, an inlet 324 for taking in the outside air ea is provided.
Is equipped with a pre-filter 326. Accordingly, the outside air ea introduced through the introduction port 324 is removed by the pre-filter 326 to remove dust, dust and the like, and is taken into the dehumidifier 304.
In 4, the dehumidifying process is performed. The dehumidified outside air is supplied to the downstream air conditioner 302 as primary air.

As shown in FIG. 14, the air conditioner 302 includes primary air a1 from the dehumidifier 304 or the inlet 710 and exhaust air from the coating equipment 14 (exhaust other than local exhaust).
mixer 33 that mixes ra and outputs as mixed air ha
0, two humidifiers 332a and 332b that perform humidification processing on the mixed air ha output from the mixer 330 and output them as secondary air a2, and secondary from the two humidifiers 332a and 332b. Air a2 application equipment 1
It has four blowers 334a to 334d that supply air to four.

The humidifiers 332a and 332b have a heating plate 336 therein for adding water vaporized to the primary air a1. Pure water is stretched over the heating plate 336. As the pure water in this case, pure water having a specific resistance of 0.15 MΩ (room temperature) or more is suitable, preferably a specific resistance of 1.5 MΩ (room temperature) or more, and more preferably a specific resistance of 15 MΩ (room temperature) or more. It is recommended to use pure water. In this embodiment, pure water having a specific resistance of 2 MΩ (room temperature) is used.

As a method for obtaining the pure water, for example, there is a method using distillation or an ion exchange resin, and a method using an ion exchange resin is preferable from the viewpoint of the efficiency of removing impurities.

On the other hand, as shown in FIGS. 9 and 10, four high-performance packed bed filters (HEPA filters) 34 are provided above the coating equipment 14 in the air supply path to the coating equipment 14.
0a to 340d are provided. In addition, between the four blowers 334a to 334d and the corresponding four supply ducts 320a to 320d,
2a to 342d are provided. These directional plates 34
Among the 2a to 342d, the first directing plate 342a corresponding to the first blower 334a located on the rightmost side in FIG.
Is connected to the second processing unit 3 through the second air supply duct 320b.
2 (see FIG. 1) is supplied to the first processing unit 30
It is installed diagonally so that it is larger than the air flow to
In FIG. 9, the fourth directing plate 342d corresponding to the fourth blower 334d located on the leftmost side is the third air supply duct 32.
The second processing unit 32 is installed obliquely so that the amount of air supplied to the second processing unit 32 through 0c is greater than the amount of air supplied to the third processing unit 34.

The second directional plate 342b corresponding to the second blower 334b is provided with a second air supply duct 320c that controls the amount of air to be supplied to the second processing unit 32 through the third air supply duct 320c. Is installed obliquely so as to be larger than the amount of air blown into the second processing unit 32 through the third processing unit 32.
The third directional plate 342c corresponding to the blower 334c of
The air flow amount supplied to the second processing unit 32 through the second air supply duct 320b is obliquely oriented so as to be larger than the air flow amount sucked into the second processing unit 32 through the third air supply duct 320c. It is installed in.

That is, the second and third air supply ducts 320b
And the amount of air supplied to the second processing unit 32 through the first air supply duct 320a and the amount of air supplied to the first processing unit 30 through the first air supply duct 320a.
0d, the first to fourth directional plates 342a to 342a to 342a to be larger than the amount of air supplied to the third processing unit 34.
The direction of 342d is set.

In the upper part of the coating facility 14, the four air supply ducts 320a to 320d and the corresponding HEPA
Directional plates 344a to 344d are provided between the filters 340a to 340d, respectively. Of these directional plates 344a to 344d, the first directional plate 344a corresponding to the first HEPA filter 340a located on the rightmost side in FIG. 9 is clean and supplied through the first air supply duct 320a. The fourth directional plate 344d corresponding to the fourth HEPA filter 340d located on the leftmost side in FIG. 9 is provided with a fourth direction plate 344d, which is obliquely installed so that the air ca is directed to the second processing unit 32 side. The clean air ca supplied through the air supply duct 320d is installed obliquely so as to be directed to the second processing unit 32 side.

The second directing plate 344b corresponding to the second HEPA filter 340b is connected to the second air supply duct 3
The third directing plate 344c corresponding to the third HEPA filter 340c is installed obliquely in a direction that suppresses all clean air ca supplied through the second processing unit 32 from being supplied to the second processing unit 32. The second processing unit 32 is provided obliquely in such a direction as to suppress all the clean air ca supplied through the third supply duct 320c from being supplied to the second processing unit 32.

The orientation of the four orientation plates 342a to 342d on the air conditioner 302 side and the orientation of the four orientation plates 344a to 344d on the application facility 14 side depend on the orientation of the coating facility 14.
The amount of air supplied to the second processing unit 32 disposed in the center of the first and third processing units 30 and 34 disposed in the periphery thereof is larger than the amount of air supplied to This allows
The pressure in the atmosphere in the second processing unit 32 is higher than the pressure in each atmosphere in the first and third processing units 30 and 34.

That is, by providing a plurality of directional plates as described above in the blowing path, the moisture in the air humidified by the air conditioner 302 is evenly mixed, and the second processing unit 3
2, the variation in humidity between the spin coaters 52 can be reduced, and the difference in wind speed between the spin coaters 52 with respect to the downward wind speed in each spin coater 52 can be eliminated.

As shown in FIG. 1, a first partition plate 70 is provided between the first and second processing units 30 and 32,
Since the second partition plate 72 is provided between the first processing unit 30 and the third processing unit 32 and the third processing unit 32,
Of air to the processing unit 32 and the third processing unit 3
4 is no longer circulated to the second processing unit 32, and the pressure in the atmosphere in the second processing unit 32 is reduced to the first pressure.
In addition, the pressure is maintained higher than the pressure in each atmosphere in the third processing units 30 and 34.

That is, the four directional plates 342a to 342d on the air conditioner 302 side and the four directional plates 3 on the coating facility 14 side
44a to 344d, and the first and second partition plates 7
0 and 72 function as air volume control means for setting the pressure in the atmosphere in the second processing unit 32 higher than the pressure in each atmosphere in the first and third processing units 30 and 34. become.

Next, the exhaust device 306 is shown in FIGS.
As shown in FIG. 3, there is provided a buffer box 500 in which the outer casing is formed in a substantially rectangular parallelepiped shape and the inside is airtight. In the buffer box 500, six exhaust blowers 502 are provided corresponding to the six spin coaters 52 in the coating equipment.

Further, between the six spin coaters 52 and the corresponding exhaust blowers 502, for example, an exhaust amount adjusting valve mechanism 508 composed of a butterfly valve 504 and a shutter 506, and the exhaust amount is electrically detected. Sensor 510 is provided for adjusting the amount of exhaust gas so that the drying conditions of the coating film can be appropriately changed.

The upper exhaust system 520 is connected to the subsequent stage of the buffer box 500. As shown in FIG. 12, the upper exhaust system 520
In addition to the exhaust of the above, the exhaust of molding equipment, post-processing equipment, and other various manufacturing equipment is performed through an outdoor blower 522 installed outdoors.

Of the many exhaust pipes in the upper exhaust system 520, six exhaust pipes 5 assigned to the coating equipment are used.
24 are connected to the buffer box 500, respectively. In this embodiment, as shown in FIG. 13, 6 extending from the upper exhaust system 520 to the coating equipment 14.
6 derived from the exhaust pipe 524 and the exhaust blower 502
The exhaust pipes 426 are separated from each other in the buffer box 500. The upper exhaust system 52
Each of the six exhaust pipes 524 extending from 0 to the coating equipment 14 is provided with a butterfly valve 526 so that the amount of exhaust to the upper exhaust system 520 can be adjusted. Are provided with butterfly valves 528 and 530, respectively, so that the amount of exhaust air to the outside can be adjusted.

The manufacturing system 10 according to the present embodiment has a reprocessing chamber 600 for performing a dye waste liquid recovery process separately from the coating facility 14 and the post-processing facility 16. A collection container 450 containing the collected dye waste liquid is carried into the reprocessing chamber 600 periodically or when necessary.

Further, the spinner head device 402 and the scattering prevention wall 404 of the spin coater 52 are carried into the reprocessing chamber 600 regularly or when necessary, for example, for maintenance. Cleaning is performed using a cleaning tank 602 (see FIG. 15) installed therein.

More specifically, as shown in FIG. 15, the spinner head device 40 is applied to the cleaning liquid contained in the cleaning tank 602.
2 and the scattering prevention wall 404 are immersed in the washing process (immersion washing). By this cleaning process, the dye adhering to the spinner head device 402 and the scattering prevention wall 404 is washed away and diffused into the cleaning liquid.

By repeating this washing treatment, the concentration of the dye in the washing liquid gradually increases, and the dye waste liquid 604
And accumulates in the cleaning tank 602.

In this embodiment, when the concentration of the dye waste liquid 604 in the cleaning tank 602 becomes equal to or higher than the concentration of the dye waste liquid 452 in the collection container 450, the cleaning tank 6
The dye waste liquid 604 in the collection container 450 is mixed with the dye waste liquid 604 in the collection container 450 to obtain a mixed dye waste liquid 606. In this case, mixing may be performed using a new container 608, and the dye waste liquid 4 in the collection container 450 may be stored in the cleaning tank 602.
52 may be added and mixed.

In the manufacturing system 10 according to the present embodiment, of the dye solution coating film formed on the substrate 202, the back surface cleaning mechanism 54 for removing the coating film adhered to the back surface of the substrate 202; It has an edge cleaning mechanism 92 for removing a portion corresponding to the outer peripheral edge of the substrate 202 in the dye solution coating film formed thereon. The waste liquid discharged from these mechanisms 54 and 92 Recovers, but separates from the dye waste liquids 452 and 604. That is, they are not mixed with the dye waste liquids 452 and 604.

The mixed dye waste liquid 606 is then subjected to a quantification step 610 for determining the contents of the dye and the anti-fading agent in the mixed dye waste liquid 606, and the concentration of the dye and the anti-fading agent in the mixed dye waste liquid 606 is determined. The dye and the anti-fading agent in the solution are reused as a regenerated dye solution 614 through a concentration adjusting step 612 in which the concentrations are adjusted so as to be more than two digits in accuracy.

The quantification step 610 may be performed by any quantification method, but is preferably quantified by liquid chromatography in consideration of the stability of the dye and anti-fading agent at the time of measurement.

In the dye concentration adjusting step 612 described below, in order to strictly adjust the concentrations of the dye and the anti-fading agent with the precision of two significant figures, it is necessary to perform the quantification with the precision of three or more significant figures. Is preferred.

In order to realize such high-precision quantification, first, as a separation condition, in the spectral absorption spectrum, each peak of the dye and the anti-fading agent does not overlap with other peaks, and each peak is a single peak. It is necessary to be. For example, liquid chromatography using an indolenine-based dye (compound A) represented by the following structural formula (A) as a dye and an anti-fading agent (compound B) represented by the following structural formula (B) as an anti-fading agent FIG. 16 shows the three-dimensional chart (representing the relative detection intensity with respect to the elapsed time after injection at each measurement wavelength).

[0129]

Embedded image

[0130]

Embedded image

The separation conditions in this case are as follows: Column: TSK-gel ODS-80Ts Column temperature: 25 ° C. Eluent: acetonitrile / water / acetic acid / triethylamine = 750/250/2/2 Flow rate: 1 ml / min Pressure: 59 bar Detection wavelength: 254 nm Sample injection amount: 20 μm.

As can be seen from FIG. 16, under these conditions, the peaks of the dye and the anti-fading agent are separated without overlapping other peaks.

Next, the detection wavelength is preferably selected so that the detection accuracy of each compound is ensured by three or more significant figures. For quantification of each compound, it is usual that a calibration curve is prepared at the detection wavelength, and the content is calculated from the detection intensity based on the calibration curve.

Therefore, in order to improve the detection accuracy of each compound, it is preferable that the calibration curve at the detection wavelength has a large correlation coefficient. Conversely, a detection wavelength exhibiting such a high correlation must be selected.

In general, the detection intensity of the dye is large, and there is no problem in the detection accuracy. Therefore, it is preferable in terms of detection accuracy to select a detection wavelength at which the detection intensity of the anti-fading agent is increased to some extent. For example, as shown in FIG. 17, when the detection wavelength is 450 nm, the correlation coefficient of the anti-fading agent is 0.999, which is a maximum at 0.999. Therefore, it is preferable to select 450 nm as the detection wavelength.

In order to perform quantification with good reproducibility, the injection accuracy of the sample is preferably 2 digits or more, more preferably 3 digits or more.

Next, in the concentration adjusting step 612, the content of the dye and the anti-fading agent in the regenerated dye solution 614 is determined based on the contents of the dye and the anti-fading agent in the mixed dye waste liquid 606 determined in the quantitative step 610. Adjust the volume.

The formulation of the preparation of the solution is not sufficient in order to fix the content of any of the dye, the anti-fading agent and the solvent and to obtain the initially adjusted concentrations of the dye and the anti-fading agent in the dye solution. The calculation is performed by calculating the amount of the movement.

The concentration of the dye and the anti-fading agent is adjusted by adjusting the concentrations of the dye and the anti-fading agent in the regenerated dye solution 614 to the concentrations of the dye and the anti-fading agent in the dye solution with a precision of two digits or more. In such a manner, in accordance with the above-mentioned calculated values, the dye and the anti-fading agent are replenished in a deficient amount and diluted with a solvent.

For example, the concentration of the dye and the concentration of the anti-fading agent in the dye solution are 2.575% by weight and 0.257% by weight, respectively.
% By weight, and when the concentrations of the dye and the anti-fading agent in the mixed dye waste liquid 606 are 6.14% by weight and 0.256% by weight, respectively, 12.284 g of dye is contained in 200 g of the mixed dye waste liquid. And the anti-fading agent is 0.512 g.

To add other components (anti-fading agent and solvent) without adding a dye and to make each component have a concentration of the dye solution, 0.714 g of the anti-fading agent and 276.34 of the solvent are used.
g must be added exactly. It is preferable to add the components other than the dye and the anti-fading agent with the same accuracy.

As described above, in the manufacturing system 10 according to the present embodiment, the dye waste liquid 6 collected in the cleaning step is used.
04 and the dye waste liquid 45 discharged in the coating process of the dye solution
2 (dye waste liquid collected in the recovery step) to obtain a mixed dye waste liquid 606, and to reuse the mixed dye waste liquid 606 as a recycled dye solution 614,
4 can be greatly increased, and the production efficiency can be improved.

In particular, the dye waste liquid 60 recovered in the washing step
The dye waste liquid 45 recovered in the above-mentioned recovery step has a dye concentration of 4
At the stage where the dye concentration becomes 2 or more, these dye waste liquids 45
2 and 604 are mixed, so that impurities can be prevented from entering the process, and the mixed dye waste liquid 606 can be prevented.
The reproducibility of the recording / reproducing characteristics can be ensured even when is reused as the reproducing dye solution 614, and the production cost can be efficiently reduced.

As a method for washing the spinner head device 402 and the scattering prevention wall 404 of the spin coater 52, the immersion washing in the washing tank 602 is performed, so that the dye waste liquid 604 is accumulated in the washing tank 602. The dye waste liquid 604 can be obtained efficiently. The immersion time in the cleaning tank 602 is preferably 10 minutes or more, and more preferably 30 minutes or more.

After the contents of the dye and the anti-fading agent in the mixed dye waste liquid 606 were quantified,
The concentration of the dye and the anti-fading agent in the dye solution is adjusted so as to match the concentration of the dye and the anti-fading agent in the dye solution with precision of two digits or more. Thus, the reproducibility of the recording / reproducing characteristics can be ensured even when reused.

In this case, as described above, it is preferable to determine the amount of the dye and the anti-fading agent in the mixed dye waste liquid 606 by liquid chromatography, and the calibration accuracy in the liquid chromatography is preferably three digits or more. .

The dye waste liquids 452 and 604 and the mixed dye waste liquid 6
06 is preferably stored in a closed container that does not transmit light. As a closed container, a stainless steel can is preferable,
More preferably, a drum made of stainless steel is desirable.

The dye waste liquids 452 and 604 and the mixed dye waste liquid 6
The storage location of No. 06 is not particularly limited as long as it is not exposed to intense light or heat, but is preferably in a building, more preferably in a room dark room. The degree of cleanliness of the storage place is less than 500,000, preferably less than 200,000.

Further, in this embodiment, the waste liquid at the time of edge cleaning and the waste liquid at the time of back surface cleaning are separated from the dye waste liquids 452 and 604, so that mixing of impurities in the mixed dye waste liquid 606 in the process can be prevented. And the mixed dye waste liquid 606
The reproducibility of the recording / reproducing characteristics can be ensured even when is reused as the reproducing dye solution 614.

The exhaust air velocity at the time of applying the dye solution is 1 m / s or less, preferably 0.7 m / s or less, more preferably 0.4 m / s or less. Thereby, the substrate 20
2 can be applied well, and the recovery rate of the regenerated dye solution 614 can be improved.

Here, preferred embodiments of other conditions will be described. The amount of the dye discharged when the dye solution is applied onto the substrate 202 is preferably 0.3 cc to 5 cc, and particularly preferably 0.5 cc to 2 cc. The temperature at which the dye solution is applied may be in the range of 10C to 50C, preferably in the range of 15C to 35C, and more preferably in the range of 20C to 25C. The temperature fluctuation in this case is in the range of ± 8 ° C., preferably in the range of ± 4 ° C., and more preferably in the range of ± 2 ° C.

The humidity at the time of applying the dye solution is 25% RH.
~ 65% RH, preferably 35% RH ~ 6.
0% RH range, more preferably 45% RH to 55% R
H range. The humidity variation in this case is in the range of ± 8% RH, preferably in the range of ± 4% RH, and more preferably in the range of ± 2% RH.

Dye recording layer 204 formed on substrate 202
Is in the range of ± 30%, preferably ± 20%, more preferably ± 15% of the normal film thickness.
% Range.

The degree of cleanliness of the substrate 202 during storage is 200,000 or less, preferably in class 10
It is less than 10,000, more preferably less than 50,000. In this case, the temperature fluctuation during storage of the substrate 202 is in the range of ± 15 ° C., preferably in the range of ± 10 ° C., and more preferably in the range of ± 5 ° C.

The light reflecting layer 208 formed on the dye recording layer 204 may be any reflecting film having a reflectance of 70% or more, but is preferably a reflecting film containing gold or silver. A reflective film of silver or gold is particularly preferred. The thickness of the light reflection layer 208 is 10 nm or more and 80
0 nm or less, and preferably 20 nm or more and 500 nm or less.

[0156]

EXAMPLES Reference Example A sealed stainless steel container was filled with 2.65 parts of the above-mentioned indolenine dye (Compound A), 0.265 parts of a fading inhibitor (Compound B), 2, 2, 3, and 3 -100 parts of tetrafluoropropanol was mixed and dissolved for 2 hours using an ultrasonic vibrator (1800 W) to prepare a dye solution for forming the dye recording layer 204.

The dye concentration in the dye solution was 2.575% by weight.
And the concentration of the anti-fading agent was 0.257% by weight.

After storing this dye solution for half a day, a spiral pregroove (track pitch 1.6 μm) was formed on the surface.
m, pregroove width 0.52 μm, pregroove depth 175 nm) of a polycarbonate substrate (diameter 120 mm, thickness 1.2 mm, manufactured by Teijin Limited, trade name “Panlite AD5503”) formed by injection molding. On the pre-groove side surface, using a spin coater 52 provided with a coating liquid applying device 400 having a nozzle made of stainless steel (inner diameter 0.8 μm), the rotation speed of the spinner head device 402 is set to 300 rpm to 4000 rpm.
The dye recording layer 204 (with a thickness of about 200 nm in the groove) was formed. The dye solution scattered at the time of application is collected through a drain 424 into a collecting container 450.
Collected.

The conditions for forming the dye recording layer 204 at this time are as follows: atmosphere temperature, humidity: 23 ° C., 50% RH dye solution temperature: 23 ° C. substrate 202 temperature: 23 ° C., exhaust air velocity: 0.8 m / s. is there.

Next, on the dye recording layer 204, Au was sputtered to form a light reflecting layer 208 having a thickness of 150 nm. Further, using another spin coater, a UV curable resin (trade name “SD-31”) is formed on the light reflection layer 208.
8 ", manufactured by Dainippon Ink and Chemicals, Inc.) while changing the rotation speed of the spinner head device from 300 rpm to 5000 rpm, and then irradiating ultraviolet rays to cure the resin, thereby forming a protective layer 210 having a layer thickness of 8 μm. Formed.

Through the above steps, an optical disk according to the reference example in which the dye recording layer 204, the light reflecting layer 208, and the protective layer 210 were laminated on the substrate 202 was manufactured.

[Example] In the above reference example, the spinner head device 402 and the scattering prevention wall 404 of the spin coater 52 are loaded into the reprocessing chamber 600 and cleaned in the cleaning tank 602. This washing process is performed by using the dye waste liquid 6
This process is repeated until the concentration of 04 becomes equal to or higher than the concentration of the waste dye 452 collected in the collection container 450.

Thereafter, the dye waste liquid 604 in the cleaning tank 602
And the dye waste liquid 452 in the collection container 450
And mixed.

The mixed dye waste liquid 60 in the another container 608
6 was placed in a 36.4 mg sample bottle, and the mixed dye waste liquid 606 was diluted with 3.0024 g of acetonitrile. On the other hand, 405.8 mg of the dye solution for forming the dye recording layer 204 shown in the reference example was placed in a sample bottle, and the dye solution was diluted with 1.204 g of acetonitrile. This was measured using liquid chromatography under the following conditions, and the concentrations of the dye (compound A) and the anti-fading agent (compound B) were quantified by the absolute calibration curve method.

The measurement conditions at this time were as follows: Column: TSK-gel ODS-80Ts Column temperature: 25 ° C. Eluent: acetonitrile / water / acetic acid / triethylamine = 750/250/2/2 Flow rate: 1 ml / min Pressure: 59 bar Detection wavelength: 254 nm Sample injection amount: 20 μm.

The dye concentration of the mixed dye waste liquid 606 is 6.92.
The concentration of the anti-fading agent was 1.139%. Based on this result, a solvent, a dye and an anti-fading agent are added so that the dye concentration and the anti-fading agent concentration match the dye concentration and the anti-fading agent concentration in the above-mentioned dye solution up to two decimal places. After adjusting the concentration, a regenerated dye solution 614 was obtained.

Using the obtained regenerated dye solution 614, the dye recording layer 20 was formed on the substrate 202 in the same manner as in the above reference example.
4. An optical disc according to an example in which the light reflecting layer 208 and the protective layer 210 were laminated was manufactured.

[Evaluation] Regarding the optical disk according to the reference example and the optical disk according to the example, “OMT” manufactured by Pulstec Inc.
Using "-2000", the recording characteristics were evaluated at the optimum power. FIG. 18 shows the result.

As is clear from FIG. 18, the optical disk D manufactured using the manufacturing system 10 according to the present embodiment, in particular, the regenerated dye solution 614 obtained by the regenerating process of the dye solution, uses a regular dye solution. There is no significant difference in the recording characteristics from the optical disk D manufactured using the same, and it can be seen that the reproduced dye solution 614 obtained in this embodiment can be reused in the dye solution coating step.

The method of manufacturing an optical information recording medium according to the present invention is not limited to the above-described embodiment, but can adopt various configurations without departing from the gist of the present invention.

[0171]

As described above, according to the method for manufacturing an optical information recording medium according to the present invention, the reproducibility of the recording / reproducing characteristics can be ensured even when the dye waste liquid is reused as the dye solution, and the manufacturing cost is reduced. Can be efficiently realized. Further, the recovery rate of the dye waste liquid can be improved, and the production efficiency can be improved.

[Brief description of the drawings]

FIG. 1 is a configuration diagram illustrating an example of a manufacturing system according to an embodiment.

FIG. 2 is a configuration diagram showing a spin coater installed in a coating facility.

FIG. 3 is a perspective view showing a spin coater installed in a coating facility.

FIG. 4 is a plan view showing a nozzle of the spin coater.

FIG. 5 is a side view showing an example of a nozzle of the spin coater.

FIG. 6 is a longitudinal sectional view showing another example of the nozzle of the spin coating apparatus with a part thereof omitted.

7A is a process diagram showing a state in which a groove is formed on a substrate, FIG. 7B is a process diagram showing a state in which a dye recording layer is formed on the substrate, and FIG. 7C is a process diagram showing a light reflecting layer on the substrate. FIG. 4 is a process diagram showing a state in which is formed.

FIG. 8A is a process diagram showing a state where an edge portion of the substrate is cleaned, and FIG. 8B is a process diagram showing a state where a protective layer is formed on the substrate.

FIG. 9 is a plan view showing an air conditioning system.

FIG. 10 is a front view showing an air conditioning system.

FIG. 11 is a side view showing the air conditioning system.

FIG. 12 is a diagram illustrating a configuration of an exhaust device in an air conditioning system together with a higher-order exhaust system.

FIG. 13 is a cross-sectional view illustrating a configuration of a buffer box installed in the exhaust device.

FIG. 14 is a block diagram illustrating a configuration of an air conditioner.

FIG. 15 is a process chart showing a reproduction process of the manufacturing system according to the present embodiment.

FIG. 16 is a view showing a three-dimensional chart of liquid chromatography using an indolenine dye and an anti-fading agent.

FIG. 17 is a table showing correlation coefficients corresponding to detection wavelengths.

FIG. 18 is a table showing recording characteristics of the optical disc according to the reference example and the optical disc according to the embodiment.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 10 ... Manufacturing system 14 ... Coating equipment 48 ... Dye coating mechanism 52 ... Spin coating apparatus 54 ... Back surface cleaning mechanism 92 ... Edge cleaning mechanism 202 ... Substrate 204 ... Dye recording layer 206 ... Edge part 300 ... Air conditioning system 400 ... Coating liquid application apparatus 402: spinner head device 404: scattering prevention wall 406: nozzle 408: discharge amount adjusting valve 424: drain 450: collection container 452: dye waste liquid 600: reprocessing chamber 602: cleaning tank 604: dye waste liquid 606: mixed dye waste liquid 608 Container 610: Determination step 612: Concentration adjustment step 614: Regenerated dye solution D: Optical disk

 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Koichi Kawai 2-10-8 Shinmeidai, Hamura-shi, Tokyo F-term in Fuji Magnedisk Corporation (reference) 2H025 AA00 AB17 AC08 BH00 EA05 4F042 AA03 AA06 BA16 CC07 CC09 CC10 CC30 5D121 AA01 EE22 EE24 EE28 EE29 GG18 GG28 GG30

Claims (9)

[Claims] 1. A method of manufacturing a heat mode optical information recording medium having a dye recording layer on which information can be recorded by irradiating a laser beam on a substrate, wherein the dye recording layer is formed while rotating the substrate. A coating step of applying a dye solution to be formed on the substrate, a collecting step of collecting a dye waste liquid discharged in the coating step, and a washing step of washing the dye adhered to the periphery during the application of the dye solution And a mixing step of mixing these dye waste liquids at a stage where the dye concentration of the dye waste liquid collected in the washing step is equal to or higher than the dye concentration of the dye solution collected in the recovery step. A method for producing an optical information recording medium, comprising recycling the mixed dye waste liquid obtained in the step as a dye solution. 2. The method for manufacturing an optical information recording medium according to claim 1, wherein said cleaning step includes a step of cleaning a device for applying a dye solution onto said substrate using a cleaning tank. A method for manufacturing an optical information recording medium, characterized by: 3. The method for producing an optical information recording medium according to claim 1, wherein, when the dye solution contains a dye and an anti-fading agent, the content of the dye and the anti-fading agent in the mixed dye waste liquid. And a step of adjusting the concentrations of the dye and the anti-fading agent in the mixed dye waste liquid to match the concentrations of the dye and the anti-fading agent in the dye solution with two or more digits of accuracy. A method for manufacturing an optical information recording medium, comprising: 4. The method for manufacturing an optical information recording medium according to claim 3, wherein the amounts of the dye and the anti-fading agent in the mixed dye waste liquid are determined by liquid chromatography. 5. The method for producing an optical information recording medium according to claim 1, wherein the degree of cleanness during storage of the mixed dye waste liquid is class 50.
A method for manufacturing an optical information recording medium, wherein the number is not more than 10,000. 6. The method for manufacturing an optical information recording medium according to claim 1, wherein the coating of the dye solution formed on the substrate has an outer peripheral edge of the substrate. A method for manufacturing an optical information recording medium, comprising separating an edge cleaning waste liquid from the dye waste liquid when the method includes an edge cleaning step of removing a corresponding portion. 7. The method for manufacturing an optical information recording medium according to claim 1, wherein a coating solution of the dye solution formed on the substrate adheres to a back surface of the substrate. A method for producing an optical information recording medium, comprising separating a waste liquid from the back surface cleaning from the dye waste liquid when a back surface cleaning step of removing a coating film is included. 8. The method for manufacturing an optical information recording medium according to claim 1, wherein an exhaust air velocity at the time of applying the dye solution is 1 m / s or less. Manufacturing method of information recording medium. 9. The method for manufacturing an optical information recording medium according to claim 1, wherein the dye solution is applied to the substrate when a dye solution is applied on the substrate to form the dye recording layer. 0.3cc to 5cc
A method for manufacturing an optical information recording medium.