JPS602901A - Method for dyeing thin film - Google Patents

Abstract

PURPOSE:To enable measurement with high accuracy without requiring cleaning and drying operations, and suspending dyeing, by measuring optical characteristics of a dyed thin film in a dyeing-stabilized transparent soln. CONSTITUTION:A thin film 2 made of a high mol.wt. substance, such as natural protein is formed on one side of a transparent glass base 1, and the obtained body to be dyed is immersed in a dyeing soln. 3 made of an acidic dye to dye it in prescribed conditions. Then, it is immersed in an acidic soln. and its light transmittance is measured there with a light guide type photometer. A light emit ting guide 5 and a light receiving guide 6 are arranged at a prescribed interval, and each of their end faces 7, 8 is opposite to each other across the body. The light transmittance is determined by measuring an amt. of light received with the guide 6, and when additional dyeing is necessary, the body is again immersed in the dyeing soln. to dye it for a time length estimated in accordance with the measured result. When it is overdyed, it is immersed in an alkaline decoloring soln. to decolor it for a estimated time.

Description

[Detailed Description of the Invention] [Field of Application of the Invention] The present invention relates to a thin film dyeing method in which a thin film deposited on a transparent substrate is dyed to have predetermined optical properties, such as when forming an optical color filter. It is related to.

[Background of the invention]

As a method for forming an optical color filter, a thin film of gelatin, casein, etc. is formed as a dyeable coating on a transparent substrate, such as a glass substrate, and the film is immersed in a dye solution containing a dye, such as an acid dye, to be dyed. A method of obtaining a transparent substrate with a thin film is known.

By the way, due to the purpose of use of such optical color filters, it is natural that the spectral transmission characteristics are an important item to keep in mind in terms of quality, and it is necessary to determine the optimal staining solution to obtain the desired spectral transmission characteristics. Of course, it is necessary to determine the material size, film thickness, and coating formation of the coating to be dyed, but even if these are selected appropriately, there are still variations in the quality of the coating material, especially natural resins such as gelatin and casein. Regarding materials, there are unstable quality at the beginning of the material and changes in ductility after dissolving and adjusting the film-forming solution.On the other hand, regarding dyeing solutions, changes in dye concentration and changes in dyeing ability of the dyeing solution occur as the solution is used. Even if staining is performed under predetermined conditions, the same staining results may not always be obtained. For this reason, the optical properties are measured as needed as the staining progresses, and the subsequent progress of the staining is judged based on the results.

In this case, optical measurements were conventionally carried out after the dyeing was stopped and the sample was washed and dried. For this reason, there are drawbacks such as an increase in the number of work hours and the possibility of damage to the coating surface during measurement.

On the other hand, as a method for constantly determining the progress of staining, for example, a method using a light guide type light meter can be considered. In other words, optical fibers or fiber bundles are placed on the dyed portion of the substrate at a slight interval, for example, approximately 1 cm, and other optical fibers are placed on the opposite side of the substrate at a similar interval. Light is irradiated from one end of the fiber, passes through the substrate to be dyed, is received at the opposite end of the fiber, and the photosensitive element placed at the other end of the light-receiving fiber is sensitized. This is a method (unknown) to know the amount of penetration and the progress of staining.

However, in this method, the amount of light absorbed by the dyeing liquid layer between the light irradiation end and the surface to be dyed, and between the opposite substrate surface and the light receiving end is much larger than the amount of light absorbed by the film to be dyed. As the light intensity decreases and the signal-to-noise ratio decreases, the error increases due to the influence of the distance between the two fiber ends of the light guide and the sample, as well as slight variations in the staining solution concentration. There is a drawback that it cannot be done.

[Purpose of the invention]

The present invention was made in view of these circumstances, and
The purpose is to measure and control the progress of staining with high precision without cutting the staining process.
- To provide a ygt staining method.

[Summary of the invention]

In order to achieve such an objective, the present invention involves dyeing under certain predetermined conditions, and then immersing the thin film in a transparent bath solution that stabilizes the dyeing. The optical properties are measured under the conditions.

The measurement of optical properties is carried out using the light guide nine-fluorescence in the same manner as described above, but since the bath liquid is transparent, the amount of light absorbed by the liquid layer is small and a sufficient amount of light can be obtained.

Based on the results of measuring the light transmittance of the dyed thin film in this manner, it is determined whether to proceed with subsequent processing, that is, whether to continue dyeing, end it there, or perform decolorization.

[Embodiments of the invention]

When a natural protein-based polymer material is used as the thin film to be dyed, the most widely used dyeing solution is an acidic solution prepared by dissolving an acidic dye in water or adding an additive.

In this case, the dyed thin film removed from the dyeing solution is immersed in an acidic solution, thereby preventing the dye from re-eluting and fixing it. On the other hand, once a dye has been dyed, immersion in an alkaline solution causes some elution, that is, discoloration of the dyed thin film. Furthermore, additional dyeing can be performed by once immersing the material in an acidic solution and then immersing it in a dyeing solution again.

Utilizing this characteristic, as shown in FIG. 1, a chromosome to be dyed, which has a dyed portion M2 made of the above-mentioned polymer substance formed on one side of a transparent glass substrate 1, is immersed in a staining liquid 3 made of an acidic dye. After dyeing under certain defined conditions, as shown in Figure 2, it is immersed in an acidic solution 4, and the light transmittance of the thin film to be dyed is measured in this acidic solution using the light guide type photometer described above. do. For this, as shown in the figure, the light guide 5 for light emission and the light guide 6 for light extraction are placed at a predetermined distance with respect to the chromosome, and the light emission end 7
It is convenient to incorporate the sample into a fixed jig so that the sample and the light-receiving end 8 face each other with the target chromosome in between, and then immerse it in each method as it is. Light emitted from the light emitting end 7, transmitted through the chromosome, and received by the light receiving end 8 is guided by the light guide 6 to an external analyzer (not shown). As a result of measuring the light transmittance based on the amount of received light, if the progress of the staining is not at the desired level and additional staining is required, the first staining is performed again.
As shown in the figure, the sample is immersed in the staining solution and dyed for the additional time estimated from the above measurement results. If the measurement results indicate excessive staining, the results are estimated from the measurement results. As shown in Figure 3, the dye is immersed in an alkaline decolorizing solution 9 for the required time to elute the dye and fade the color, or for more precise control, the light transmittance is further measured midway. The desired optical properties are obtained by performing elution operations as the process progresses. Depending on the case, these light transmittance measurements and additional staining or bleaching operations are repeated. If the measurement results show the desired optical characteristics, the dyeing is completed, and as shown in FIG. 4, the needle is immersed in a cleaning solution 10 for cleaning and then dried.The light guide type optical sewing needle as described above is dried. In contrast, in the method of measuring in a staining solution using a dye, effective measurements could not be performed due to light absorption due to the coloring of the staining solution, whereas in this method, measurement is performed in a bath solution that is almost optically clear, so high S /N ratio can be measured with high precision. In addition, alkaline fading liquid 9
Even when measuring during discoloration, the liquid is transparent, so highly accurate measurements can be made as well.

An example of a comparison of photometric quantities using the two-sided method is as follows:
In an example in which the thin film 2 to be dyed has a light transmittance of 50% at a specific characteristic control wavelength of the optical color filter,
The light transmittance of the staining solution is 1 per liquid layer at the above wavelength.
If it is 0%, and the distance between the light emitting end 7 and light receiving end 8 of the light guide and the chromosome to be detected is 1πm, then
Even if we assume that the light loss between the light emitting end and the light receiving end is only due to absorption by the staining solution and the thin film 2 to be dyed, and there is no other light diffusion, φ scattering, etc., in the case of the former, the amount of received light will be the same as that at the initial stage of dyeing. It accounts for 1% of the irradiated light at the final stage, and only 0.5% at the final stage. In contrast, in the case of this method, since there is almost no absorption by the liquid, the amount of light received is 100% at the initial stage of staining and 50% at the final stage, and it is clear that highly accurate measurement is possible.

It goes without saying that the acidic solution 4 must not have severe properties such as corrosive or oxidizing the material, but a volatile weak acid such as an acetic acid aqueous solution is preferable in order to avoid deterioration after completion.

In addition, as the decolorizing liquid 9, for the purpose of acidic dye elution,
Likewise suitable is an aqueous ammonia solution as a volatile weak alkali. Furthermore, it goes without saying that the dye may be simply eluted with water.

Further, in order to obtain the stability of the acidic bath solution or the discoloration solution, it is also effective to dissolve ammonium acetate in each solution.

It goes without saying that the light guide type light meter may be a simple light meter, a monochromatic photometer, or a spectrophotometer depending on the purpose of the optical color filter.

The above describes the case of dyeing a thin film made of natural protein-based polymer material for the production of optical filters, but the present invention is not limited to this, and generally dyes a thin film formed on a transparent substrate. In the case of dyeing by immersing the thin film in a liquid, a similar effect can be obtained by measuring the optical properties of the thin film in a transparent bath liquid that stabilizes the dyeing.

〔Effect of the invention〕

As explained above, according to the present invention, by adopting a method of measuring the optical properties of a thin film to be dyed in a transparent bath solution that stabilizes the dyeing, when measuring in a dyeing solution, it is possible to In contrast, a sufficient amount of light can be obtained, and high-precision measurements can be easily performed, and -1
It is not necessary to stop the dyeing operation at every stage and perform washing and drying. In particular, if the two light guides DiM that make up the light meter and the target chromosome are assembled into a jig with a fixed positional relationship, it will be extremely easy to link the two light guides and the target chromosome. There is an advantage that a highly efficient and high quality optical filter etc. can be obtained without the need to match the positional relationship between the two and without the risk of damaging the thin film at that time.

[Brief explanation of the drawing]

FIGS. 1 to 4 are diagrams for explaining one embodiment of the present invention. 1... φ glass substrate (transparent substrate), 2... Thin film to be dyed, 3... Staining liquid, 4... Acidic bath liquid, 5...
・Light guide for writing light output, 6 Light guide for light extraction, 7... Light output end, 8... Light receiving end, 9
・OS・Decolorizing liquid, 10...Cleaning liquid. Figure 1 Figure 2 Figure 3 Figure 4

Claims (1)

[Claims] 1. In a thin film dyeing method in which a thin film deposited on a transparent substrate is immersed in a dyeing solution to dye the thin film to have predetermined optical properties, the thin film is immersed in the dyeing solution and dyed. After this, the thin film is transferred to a transparent bath solution that stabilizes the dyeing, and the optical properties of the thin film are measured in the solution, and based on the measurement results, it is decided whether to continue dyeing, terminate it, or immerse it in a decolorizing solution. 'R membrane staining method, which is characterized in that it is determined whether decolorization is performed or not. 2. Thin J1et is made of natural protein-based polymer material,
The staining solution is an acidic dye aqueous solution or an aqueous solution containing additives), the transparent substrate is not made of glass or a transparent polymeric substance that does not react with the dyeing solution, and the bath solution used for measurement is a dilute acidic solution. 2. The thin film dyeing method according to claim 1, wherein the decolorizing liquid is water or a dilute alkaline liquid containing water as a main liquid.