JP2000044811A - Ultrafine particle dispersed optical material - Google Patents

Abstract

(57) [Summary] [Problem] It is difficult to easily control the light refractive index with organic optical device materials, and it is difficult to control photosensitivity such as photocurability, viscosity, etc. in printing, thin film production, pattern formation, etc. It solves the problem that it is difficult to control important characteristics easily. Kind Code: A1 Abstract: A metal powder or a metal oxide powder has a thickness of 5 nm.
Ultrafine particles pulverized so as to have a particle diameter of about 100 nm are dispersed and mixed in a resin binder, and the light refractive index is controlled by adjusting the concentration of the ultrafine particles.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an optical material capable of arbitrarily setting a refractive index of light used for an optical lens, a prism, an optical waveguide, an optical fiber, and the like.
In particular, the present invention relates to an ink-like substance in which ultrafine particles of a metal or metal oxide having a large refractive index are dispersed in an organic resin binder or an inorganic binder.

[0002]

2. Description of the Related Art Materials having a large light refractive index and materials whose light refractive index can be set arbitrarily are extremely important as materials for optical devices, and various materials are used. Materials are used.

As materials for optical devices, the use of organic materials has been studied and put to practical use because of their advantages such as easy handling, easy thin film formation and pattern formation. . For example, polymethyl methacrylate (PMMA), polycarbonate (PC), polystyrene (PS), polyurethane (P
U), polyimide (PI) and the like.

However, the light refractive index of these materials is 1.
It is in the range of about 4 to 1.7, and since these are organic substances, it is difficult to control their light refractive indexes. This is because the light refractive index is determined by the elements constituting these materials.

[0005]

With the above-mentioned materials for organic optical devices, it is difficult to easily control the refractive index of the light, and it is difficult to control the light sensitivity and photosensitivity such as photocurability and the like. It is also difficult to easily control important characteristics in thin film production, pattern formation, and the like, and the present invention has been made to solve such problems.

[0006]

The present invention is characterized in that ultrafine particles obtained by pulverizing a metal powder or a metal oxide powder so as to have a particle diameter of 5 to 100 nm are dispersed and mixed in a resin binder. Ultrafine particle dispersed optical material.

[0007] The present invention also relates to the ultrafine particle-dispersed optical material according to the above invention, wherein the ultrafine particles are contained in the range of 0.1 to 60% by weight based on the resin binder. is there.

[0008] The present invention also relates to the ultrafine particle-dispersed optical material according to the above invention, wherein the metal component of the metal powder or the metal oxide powder is titanium.

The present invention also provides the ultrafine particle-dispersed optical material according to the above invention, wherein the metal component of the metal powder or the metal oxide powder is silicon.

[0010] The present invention also relates to the ultrafine particle-dispersed optical material according to the above invention, wherein the metal component of the metal powder or the metal oxide powder is zinc.

The present invention also relates to the ultrafine particle-dispersed optical material according to the above invention, wherein the metal component of the metal powder or the metal oxide powder is aluminum.

The present invention also provides the ultrafine particle-dispersed optical material according to the above invention, wherein the metal component of the metal powder or the metal oxide powder is magnesium.

[0013] The present invention also relates to the ultrafine particle-dispersed optical material of the above invention, wherein the metal component of the metal powder or the metal oxide powder is calcium.

The present invention also relates to the ultrafine particle-dispersed optical material of the above invention, wherein the metal powder or the metal oxide powder has a light refractive index of 1.5 to 2.5.

[0015]

BEST MODE FOR CARRYING OUT THE INVENTION The ultrafine particle-dispersed optical material of the present invention is obtained by pulverizing various metal powders or metal oxide powders into extremely fine ultrafine particles, and then combining an organic binder or an inorganic binder with a solvent. This is an ultrafine particle-dispersed optical material, which is used as a paint for forming a thin film or pattern.

The light refractive index of a thin film or a pattern produced by using the ultrafine particle-dispersed optical material of the present invention can be adjusted by adjusting the content of a metal or metal oxide having a large refractive index as a dispersoid. Control and the amount of organic binder or inorganic binder and solvent, dispersion state,
The dispersion conditions and the like control various properties required for coating and printing suitability, thinning, and pattern production, such as the viscosity and photocurability of the optical material as the coating material.

The above two optical materials, that is, ultrafine metal particles and ultrafine metal oxide particles capable of controlling the light refractive index, and an organic or inorganic binder are mixed and uniformly monodispersed to form a composite. By doing so, it is possible to easily control the refractive index arbitrarily and to constitute an optical material as a coating material having characteristics required for thinning or pattern formation.

[0018]

EXAMPLES The ultrafine particle-dispersed optical material of the present invention will be described below in detail based on specific examples.

Example 1 Titanium oxide powder (manufactured by Kanto Chemical Co., Ltd.) as a metal oxide and polymethyl methacrylate (PMMA; Mitsubishi Rayon Co., Ltd.) as a binder resin
MT-1 (manufactured by ICI Japan), cyclohexanone (Wako Pure Chemical Industries, Ltd.) as a binder solvent
Was mixed with the composition shown in Table 1 (paint A, paint B, paint C) and then crushed into ultrafine particles using a crusher according to the following procedure to disperse ultrafine titanium oxide particles. The ultrafine particle-dispersed optical material of the present invention is produced.

[0020]

[Table 1]

First, the raw materials mixed in the configuration shown in Table 1 are
Using a pulverizer (Eiger Mill; manufactured by Eiger Japan Co., Ltd.), a pulverizing treatment and a dispersing treatment are performed for 350 hours, and paint A, paint B, paint C in which extremely fine ultrafine titanium oxide particles are monodispersed are used. An ultrafine particle-dispersed optical material of the present invention was produced.

As a result of observing the ultrafine particles of titanium oxide in the obtained paints A, B and C by using an atomic force microscope, the ultrafine particles of titanium oxide were pulverized to a size of about 20 to 30 nm. Was dispersed.

Then, the obtained paints A, B, C
Was applied on a smooth transparent glass substrate to prepare test pieces on which thin films Aa, Bb, and Cc were formed by paints A, B, and C, respectively. Then, each thin film A on the test piece
As a result of observing the light scattering states of a, Bb, and Cc, all were thin transparent films without light scattering.

For each of the obtained thin films Aa, Bb, and Cc, the light refractive index (refractive index at a light wavelength of 1300 nm) was measured, and the titanium oxide concentration (% by weight) of each of the thin films Aa, Bb, and Cc was measured. A graph showing the relationship with the light refractive index was prepared. FIG. 1 is a graph showing the relationship between the photorefractive index of each of the thin films Aa, Bb and Cc and the concentration of titanium oxide (% by weight). The relationship between the two is included in the range of two line graphs in FIG. ing.

As shown in FIG. 1, each thin film Aa, Bb, C
The refractive index of c increases as the concentration of titanium oxide having a large refractive index increases, and the light refractive index of the formed thin film can be easily controlled by adjusting the concentration of ultrafine titanium oxide in the thin film. I found that I could do it.

Example 2 Titanium oxide powder (manufactured by Kanto Chemical Co., Ltd.) as a metal oxide, a photocurable resin (SP-1509; manufactured by Showa Kogaku KK) as a binder resin, Hyperma MT-1 ( Cyclohexanone (manufactured by Wako Pure Chemical Industries, Ltd.) as a binder solvent,
After mixing according to the composition shown in Table 2 (Paint D, Paint E, and Paint F), the mixture was crushed into ultrafine particles using a crusher according to the following procedure, and the ultrafine particles of the present invention in which ultrafine particles of titanium oxide were dispersed were used. A fine particle-dispersed optical material is produced.

[0027]

[Table 2]

First, the materials mixed in the configuration shown in Table 2 were
Using a pulverizer (Eiger Mill; manufactured by Eiger Japan Co., Ltd.), a pulverization treatment and a dispersion treatment for 150 hours were carried out, and three types of photocurable paints D, E and F in which ultrafine ultrafine titanium oxide was monodispersed. Of the present invention was produced.

Then, each of the obtained photocurable paints D, E, and F is applied on a smooth transparent glass substrate, and each photocurable thin film Da, E,
b, a test piece on which Fc was formed was prepared.

Then, using the negative pattern mask of the test pattern shown in FIG. 2, the film surface of each photocurable thin film Da, Eb, Fc of the test piece was subjected to pattern exposure with ultraviolet light,
The exposed portions are photopolymerized and cured, and the unexposed portions are dissolved and developed and removed with a cyclohexanone solvent, and the thin films Da, Eb, and Fc are removed.
Each pattern shown in FIG. 2 was formed.

Then, the obtained thin films Da, Eb, Fc
As a result of observing the ultrafine particles of titanium oxide in the respective patterns by using an atomic force microscope, the ultrafine particles of titanium oxide were pulverized and dispersed to a size of about 20 to 30 nm. Then, each thin film Da, E on the test piece
As a result of observing the light scattering state of the pattern portion due to b and Fc, each was a transparent thin film without light scattering.

For each of the obtained thin films Da, Eb, and Fc, the light refractive index (refractive index at a light wavelength of 1300 nm) was measured, and the titanium oxide concentration (% by weight) of each of the thin films Da, Eb, and Fc was measured. A graph showing the relationship with the light refractive index was prepared. FIG. 3 is a graph showing the relationship between the photorefractive index of each of the thin films Da, Eb, and Fc and the titanium oxide concentration (% by weight), and the relationship between the two is included in the range of two line graphs in FIG. ing.

As shown in FIG. 3, each thin film Aa, Bb, C
The refractive index of c increases as the concentration of titanium oxide having a large refractive index increases, and the light refractive index of the formed thin film can be easily controlled by adjusting the concentration of ultrafine titanium oxide in the thin film. I found that I could do it.

[0034]

The ultrafine particle-dispersed optical material of the present invention has a high refractive index contained in the thin film obtained by coating the thin film or the patterned thin film formed by patterning the thin film. By adjusting the concentration of the ultrafine particles of a metal or metal oxide having a low refractive index, there is an effect that the refractive index can be controlled so as to have an appropriate refractive index.

The ultrafine particle-dispersed optical material of the present invention has a function as a photosensitive ultrafine particle-dispersed optical material for forming a pattern by a lithography method by using a photocurable resin as a binder resin. It is possible.

As described above, the ultrafine particle-dispersed optical material of the present invention can easily control the refractive index of a high refractive index thin film or a thin film pattern and easily form a high refractive index thin film pattern, which has been conventionally difficult. There is an effect that can be.

[Brief description of the drawings]

FIG. 1 is a graph showing a relationship between a titanium oxide concentration (% by weight) and a photorefractive index of a thin film formed by the ultrafine particle-dispersed optical material of the present invention.

FIG. 2 is a plan view showing an example of a thin film pattern formed by using the photosensitive ultrafine particle-dispersed optical material of the present invention.

FIG. 3 is a graph showing a relationship between a titanium oxide concentration (% by weight) and a photorefractive index of a thin film formed of the photosensitive ultrafine particle-dispersed optical material of the present invention.

Claims (9)

[Claims] 1. A metal powder or a metal oxide powder having a thickness of 5 nm.
An ultrafine particle-dispersed optical material, wherein ultrafine particles pulverized so as to have a particle size of 1 to 100 nm are dispersed and mixed in a resin binder. 2. The ultrafine particle-dispersed optical material according to claim 1, wherein said ultrafine particles are contained in an amount of 0.1 to 60% by weight based on the resin binder. 3. The ultrafine particle-dispersed optical material according to claim 1, wherein the metal component of the metal powder or the metal oxide powder is titanium. 4. The ultrafine particle dispersed optical material according to claim 1, wherein the metal component of the metal powder or the metal oxide powder is silicon. 5. The ultrafine particle-dispersed optical material according to claim 1, wherein the metal component of the metal powder or the metal oxide powder is zinc. 6. The ultrafine particle dispersed optical material according to claim 1, wherein the metal component of the metal powder or the metal oxide powder is aluminum. 7. The ultrafine particle-dispersed optical material according to claim 1, wherein the metal component of the metal powder or the metal oxide powder is magnesium. 8. The ultrafine particle dispersed optical material according to claim 1, wherein the metal component of the metal powder or the metal oxide powder is calcium. 9. The ultrafine particle-dispersed optical material according to claim 1, wherein the metal powder or the metal oxide powder has a light refractive index of 1.5 to 2.5.