KR100201867B1 - Manufacturing method of ray-sensitive glass by sol-gel method - Google Patents

Abstract

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to photosensitive glass manufactured by the sol-gel method and a method of manufacturing the same. The present invention relates to a photosensitive glass produced by a simple step of coating a film, a method of manufacturing the same, and a method of forming a pattern thereon.

Description

Photosensitive glass by sol-gel method and its manufacturing method

FIG. 1 is a process chart showing a process of preparing a photosensitive glass and forming a pattern by a sol-gel method.

The present invention relates to a photosensitive glass produced by a sol-gel method and a method of manufacturing the same. More specifically, a photosensitive sol (Sol) is applied to a glass substrate to form a pattern such as a semiconductor or a liquid crystal display (LCD). It relates to a photosensitive glass produced by a simple step of coating, a method for producing the same, and a method for forming a pattern therein.

The photosensitive mechanism of photosensitive glass is such that when Ce ^{+ 3} in the glass is irradiated with UV light, Ce ⁺³ releases one electron, which is absorbed by Ag ⁺ so that Ag ^o colloid is formed to exist as a nucleus for crystallization. As a result, the crystallization of the glass is facilitated even at the heat treatment at a lower temperature than the non-exposed portion without the nucleus for crystallization.

Conventionally proposed methods for producing such photosensitive glass are US Patent Nos. 2,515,936, 2,515,937, 2,515,939, 2,515,940, 2,515,941, 2,515,943, 2,651,146, etc. The method is, for example, by adding cerium, antimony as a sensitizer and additives such as copper, gold, silver and the like as a sensitizer to sodium silicate glass or lithium lithium silicate glass and producing photosensitive glass by melting.

However, in the case of manufacturing photosensitive glass by the conventional melting method, a large amount of energy is required for high temperature melting, there is a high probability that impurities may be mixed, and it is difficult to highly homogenize the glass, and also by melting the glass Since the mold had to be manufactured, it could not be coated using other materials as the substrate.

Accordingly, an object of the present invention is to provide a photosensitive glass that can be produced at a low temperature without solving the above problems and melting the glass at a high temperature.

Another object of the present invention is to provide a method of forming a pattern on photosensitive glass in a single process.

In order to achieve the above object, the present inventors synthesize the photosensitive sol using the sol-gel method and then perform the drying and sintering process to obtain the photosensitive glass, The present invention was completed by knowing that a pattern can be formed by a single process by coating a photosensitive sol instead of Cr coating and photoresist (PR) on a substrate during a photo1ithography process for pattern formation. .

Hereinafter, the present invention will be described in detail.

The present invention is a network-forming material of the Si0 ₂ -alkoxide compound 69.45 to 90.5 mol%, alkali compounds 9.45 to 30.5 mol%, 0.003 to 0.7 mol% of the photosensitive agent and 0.01 to 1.5 mol% of the photosensitive agent are mixed and an alkoxide compound sol of the photosensitive glass of characterized in that of 2.2 times to 10 times of ethanol and H ₂ 0 in the mixture is based on to be characterized.

Such a method of manufacturing the photosensitive glass of the present invention, Si0 ₂ - mixing the alkoxide compound 69.45 to 90.5 mol%, the alkali compound 9.45 to 30.5 mol%, the light-sensitive claim 0.003 to 0.7 mol and the light-sensitive agent from 0.01 to 1.5 mol% And adding 2.2 times ethanol and 10 times H ₂ 0 based on the alkoxide compound,

Vigorously stirring and mixing the mixture to synthesize a photosensitive sol,

Immersing and coating a substrate in the photosensitive sol, and

The coated substrate material is dried and subjected to a sintering process at about 400 ° C.

In addition, the method of forming a pattern on the photosensitive glass thus prepared further comprises the step of partially exposing the substrate coated with the photosensitive glass to UV light and heat-processing to about 500 ° C. after the manufacturing process of the photosensitive glass is completed. By carrying out it can be completed in a single process.

The present invention will be described in more detail as follows.

The present invention relates to a photosensitive glass prepared in detail by a sol-gel method and a method for manufacturing the same, wherein the photosensitive glass of the present invention is 69.45 to 90.5 mol%, an alkyl compound of a SiO ₂ -alkoxide compound which is a network forming material. 9.45 to 30.5 mol%, 0.003 to 0.7 mol of the photosensitizer and 0.01 to 1.5 mol% of the photosensitizer are mixed, and vigorously stirred by adding 2.2 times ethanol and 10 times H ₂ O based on the alkoxide compound. A photosensitive sol is synthesized and immersed and coated on a substrate, followed by drying and sintering.

A service source that causes the Si0 ₂ network structure herein tetraethylorthosilicate _{[TEOS, Si (OC 2 H} 5) 4] , it is preferable to use a distilled water and ethanol to form a Si0 ₂ network, as the alkaline compound Lyrium providing a source to use a Lyrium isopropoxide (LiOC ₃ H ₇₎ preferred bar, these two elements are the reason is used for crystallization of glass selected a composition range as described above Si0 _2- Li ₂ 0 in the glass-based This is because the composition range of the spinoidal decomposition region that may cause crystallized glass.

In addition, the light-sensitive first as the cerium nitrate (Ⅲ) · 6 hydrate _{[Ce (NO 3) 3 ·} 6H 2 O] is Examples of preferred, and photo sensitive agent of silver nitrate (AgNO ₃₎ used for producing the photosensitive glass of the present invention desirable. At this time, excessive use of the photosensitizer or the photosensitizer is not preferable because it is difficult to maintain the charge neutrality of the Si0 ₂ network structure and silver or cerium precipitates.

As another method for producing the photosensitive glass of the present invention, lithium acetate may be used as the alkali compound or cerium chloride may be used as the photosensitive agent.

Production method of the photosensitive glass of the present invention, Si0 ₂ - alkoxide compound 69.45 to 90.5 mol%, the alkali compound 9.45 to 30.5 mol%, the light-sensitive claim 0.003 to 0.7 mol and the light-sensitive mixed agent 0.01 to 1.5 mol%, and the Adding 2.2 times ethanol and 10 times H ₂ 0 based on the alkoxide compound,

Vigorously stirring and mixing the mixture to form a photosensitive sol,

Immersing and coating a substrate in the photosensitive sol, and

The coated substrate material is dried and subjected to a sintering process at about 400 ° C.

By going through such a step, it is possible to manufacture the high purity high homogeneous photosensitive glass of the present invention at a low temperature.

Furthermore, the method for forming a pattern on the photosensitive glass-coated glass substrate of the present invention may be performed by partially exposing the substrate coated with the photosensitive glass to UV light after the above-described photosensitive glass manufacturing process is completed. This is terminated by further performing the step of heat treatment at ° C.

In this manner, a high homogeneous and high purity photosensitive glass could be produced at a low temperature by the sol-gel method, and in particular, coating could be performed using the photosensitive sol.

This process of the present invention is as shown in FIG.

After coating, heat treatment is performed to form a metasilicate crystal phase. Since the crystal phase is about 30 to 50 times faster than the glass of the non-exposed part, the pattern can be formed by partial etching. The coating process of Cr and photoresist during the photomark manufacturing process of semiconductors and LCDs can be simplified into a single process using photosensitive coating glass by photosensitive sol coating.

Hereinafter, the present invention will be described in more detail with reference to Examples, which are not intended to limit the present invention in any way.

Example 1

In a three-necked flask, 0.32 g of tetraethoxy orthosilicate (TEOS), lithium isopropoxide (0.025 g), 3 ml of ethanol and 15 ml of water were mixed, and cerium nitrate (III) hexahydrate 1.01. 0.015 g of g and silver nitric acid were added and mixed with vigorous stirring.

The microscope slide glass (2 inches x 1 inch x 1.1 mm) was immersed in the photosensitive sol thus prepared, and then dried in air.

Then, a sintering process was performed at about 400 ° C. for 2 hours to coat the photosensitive glass on the slide glass.

The resulting photosensitive glass-coated-slide glass was partially exposed to UV light using a UV irradiator and heat treated at 500 ° C.

As a result, it was confirmed that crystallized glass, which is a metathium silicate (Li ₂ Si0 ₃ ), was formed on the part exposed to UV light, and the non-exposed part remained glassy.

Example 2

The same procedure as in Example 1 was repeated, except that cerium chloride was used in place of cerium nitrate hexahydrate, and lithium acetate was used in place of lithium isopropoxide. As a result, the same product as in Example 1 was obtained.

Example 3

The same method as in Example 1 was repeated, but lithium acetate was used instead of lithium isopropoxide. As a result, the same product as in Example 1 was obtained.

Claims (8)

In photosensitive glass, Si0 ₂ - network-forming material is Si0 ₂ - alkoxide compound 69.45 to 90.5 mol%, the alkali compound 9.45 to 30.5 mol%, the light-sensitive claim 0.003 to 0.7 mol%, and a light-sensitive agent from 0.01 to 1.5 mol, A photosensitive glass, wherein the substrate is immersed in a photosensitive sol, in which% is mixed with 2.2 times ethanol and 10 times H ₂ O based on the alkoxide compound, and dried and sintered. The photosensitive glass according to claim 1, wherein the alkoxide compound is tetraethyl orthosilicate. The high purity photosensitive glass according to claim 1, wherein the alkali compound is lithium isopropoxide or lithium acetate. The photosensitive glass according to claim 1, wherein the photosensitive agent is cerium nitrate (III) hexahydrate [Ce (N0 ₃ ) ₃ .6H ₂ 0] or cerium chloride. The photosensitive glass according to claim 1, wherein the photosensitive agent is silver nitrate (AgN0 ₃ ). Preparing a sol composed of a raw material, synthesizing a photosensitive sol, coating the synthesized sol on a glass substrate, drying and sintering the coated glass substrate, and sintering the sintered glass substrate. Method for producing a photosensitive glass, characterized in that it comprises a step of forming a pattern. The photosensitive sol of claim 6, wherein the photosensitive sol comprises: 69.45 to 90.5 mol% of a SiO ₂ -alkoxide compound, 9.45 to 30.5 mol% of an alkali compound, 0.003 to 0.7 mol of a photosensitive agent, and 0.01 to 1.5 mol% of a photosensitive agent, Method for producing a photosensitive glass, characterized in that consisting of 2.2 times ethanol and 10 times H ₂ 0 based on the alkoxide compound. The method of claim 6, wherein the pattern forming step includes a step of partially heat-treating the coated substrate to UV light.