JPH02120246A - Manufacturing method of fine pattern transfer glass - Google Patents

Abstract

(57) [Abstract] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing a glass molded article having fine bubbles.

[Prior Art] Methods for manufacturing glass molded products having fine patterns include methods using electron beam drawing and machining.

However, all of these methods require large-scale and expensive equipment, have complicated and long steps, and have low throughput. In order to overcome these drawbacks, a pattern transfer method using a sol-gel method has been proposed. (
JP-A-6O-21215r Fine pattern fabrication method”)
[Problem to be Solved by the Invention 1] However, the pattern transfer glass obtained by this method suffers from deformation caused by uneven drying speed when drying the wet gel.
1 due to deformation caused by uneven shrinkage rate during sintering.
For example, the flatness deteriorates, resulting in poor molding accuracy.The present invention was made to solve the above problems, and its purpose is to provide a pattern with excellent molding accuracy. The objective is to produce transfer glass by a sol-gel method.

[Means for solving the problems] The first method for manufacturing fine pattern transfer glass of the present invention includes:
After preparing a liquid sol having a desired glass component composition using one or more metal alkoxides as main raw materials, and gelling the liquid sol while contacting a matrix having a desired shape or pattern to produce a wet gel, A method for producing fine pattern transfer glass by a sol-gel method in which the wet gel is vitrified by heat treatment such as drying and sintering, characterized in that the wet gel is dried under supercritical conditions.

Further, a second method of manufacturing fine pattern transfer glass of the present invention is a method of manufacturing fine pattern transfer glass using a sol-gel method, characterized in that the wet gel is dried in a liquid.

A third method of manufacturing fine pattern transfer glass of the present invention is a method of manufacturing fine pattern transfer glass using a sol-gel method, characterized in that the wet gel is lowered into the air and dried.

A fourth method for producing fine pattern transfer glass of the present invention is a method for producing fine pattern transfer glass according to item 1, 2, or 3, in which dry gel obtained by drying the wet gel is sintered. When sintering, the dry gel is sintered while applying a load so as to follow the shape of the dry gel base.

Further, the fifth method of manufacturing a fine pattern transfer glass of the present invention includes a liquid having a target glass component composition used in the method of manufacturing a fine pattern transfer glass described in item 1 or 2 or 3 or 4. One or two types of sol f! It is characterized in that it is prepared using the above metal alkoxide and metal oxide fine particles as main raw materials.

[Function 1] The present invention will be explained in detail. When producing a glass body by the sol-gel method, deterioration in molding accuracy occurs in the wet gel drying process and the dry gel sintering process. In the drying process, since the drying air is not uniform around the wet gel, the rate of shrinkage of the wet gel varies depending on the area, resulting in deterioration of molding accuracy. Also, in the sintering process, deterioration of molding accuracy occurs due to the same reasons as the drying process and the density distribution of the dry gel constituent particles generated in the drying process.Therefore, in order to prevent this, it is necessary to It is necessary to take measures. The first method in the drying step is to perform drying under supercritical conditions using an autoclave. When wet gel is dried by this method, there is almost no shrinkage of the gel body, so deterioration of molding accuracy in the drying process can be prevented. A second method is to dry the wet gel in a liquid. Liquids can have a smaller temperature distribution than gases. At this time, the liquid must have little reactivity with the gel body, be hydrophobic, and have a low vapor pressure since heating is performed at a temperature of 60° C. or higher. As such a liquid, perfluoropolyether (-CF-CFz-0-)n (trade name: Fluorinert, manufactured by 3M Company) is preferable.A third method is to lower the wet gel into the air and dry it. It will be done. This is to prevent the wet gel from drying while in contact with some kind of base, which would result in a difference in drying speed between the surface in contact with the base and other surfaces, resulting in deterioration of molding accuracy. For this purpose, holes 41 and supporting parts 42 are formed in the gel body during molding, as shown in FIG.
It is good to set up

Next is the sintering process. At this time, a load 41 as shown in FIG. It is necessary to use materials such as alumina and stone pods that are resistant to high temperatures for both the base and the base. Also, care must be taken to avoid direct contact between the transfer section and the load.

(Example-1) S i (oct Hs) 4 208 g, 0.0
147 g of 2N hydrochloric acid was mixed and stirred to obtain a hydrolyzed solution.

40 g of S i Oa fine particles (trade name: Rheolo Seal, manufactured by Tokuyama Soda Co., Ltd.) were added and dispersed in 170 g of this hydrolyzed liquid to obtain a sol. The pH was adjusted to 4.9 by adding ammonia water to this sol, and then a mold 11 having a grouped optical disk shape, whose planar shape is shown in FIG. 1(a) and its cross-sectional shape is shown in FIG. prepared. This mold 11 was manufactured taking into account shrinkage of the gel, and the group pitch 12 was 3.2 μm, the group width 13 was 1.6 μm, and the group depth 14 was 0.16 μm. Note that FIG. 1 is exaggerated for ease of explanation. A pH-adjusted sol was poured into this mold 11 to obtain a wet gel. This wet gel was placed in an autoclave filled with ethyl alcohol of 100% by volume or more, and heated at 8000ps 1-300℃ (temperature increase rate 50℃/hr, pressure reduction rate 500ps i/30m).
Supercritical drying was carried out under the following conditions: 1 n).

The obtained dry gel was sintered at a maximum temperature of 1200° C. by applying a load as shown in FIG. As a result, a grouped glass disk 15 was obtained. Group pitch 16 is 1.6μm Group width 17 is 0.8u
m, group cleanliness 18 was 0°08 um, and the pattern of type 11 was faithfully reduced to 1/2. The flatness of this grouped glass disk was 24 μm.

(Example-2) A sol was obtained in the same manner as in Example-1, and after adjusting the pH, the sol was poured into a mold having the same grouped glass disk shape as that used in Example-1, and the wet gel was Obtained. The obtained wet gel was immersed in perfluoropolyether (-CF2-CF, -0-) (trade name, manufactured by Fluorinert 3M), and the perfluoropolyether was
Drying was performed by heating to 0°C. Since the obtained dry gel contains a large amount of perfluoropolyether in the bore, it
After heat treatment was carried out at 1200°C for 3 hours to sufficiently volatilize the perfluoropolyether, sintering was carried out at a maximum temperature of 1200°C. As a result, a glass disk with groups was obtained. The flatness of this grouped glass disk is 31um
Met.

(Example-3) Ss (QCs Hs)-166.4g, CH-
35.6 g of 3i (OCa Hs )z and 147 g of 0.02N diluted hydrochloric acid were mixed and stirred to obtain a hydrolyzed solution.

49 g of Si 02 fine particles (trade name: Rheolo Seal, manufactured by Tokuyama Soda Co., Ltd.) were added and dispersed in the hydrolyzed solution to obtain a sol.

Ammonia water was added to this sol to adjust the pH to 49, and this was poured into a mold having the same grouped glass disk shape as that used in Example-1 to obtain a wet gel. This wet gel was hung in a drying container and dried as shown in FIG. The obtained dry gel was heated to a maximum temperature of 120℃ in exactly the same manner as described in Example-1.
Grouped glass disks were obtained by sintering at 0°C. The flatness of this grouped glass disk is 2
It was 0 μm. On the other hand, the flatness of the grouped glass disk produced by drying the wet gel by placing the wet gel directly on the base and applying no load during sintering was 300 μm.

[Effects of the Invention] As described above, according to the present invention, in the production of fine pattern transfer glass by the sol-gel method, drying of wet gel is carried out under supercritical conditions in a liquid or in the air. By sintering the dried gel while applying a load, it is possible to obtain fine pattern-transferred glass with extremely excellent molding accuracy. It goes without saying that this method can be applied not only to the example described in this embodiment, but also to the production of gratings, holographic elements, lenses, waveguide elements, various glass substrates, and the like.

[Brief explanation of the drawing]

FIGS. 1(a) and 1(b) are diagrams explaining the shape of the matrix used in the first embodiment of the present invention, and FIG. 1(c) is a group obtained in the first embodiment of the present invention. 2 is an explanatory diagram of how to apply a load used in the first embodiment of the present invention. FIG. 3 is an explanatory diagram of the drying method of the third embodiment of the present invention. Figures 4 (a) and (b) are explanatory diagrams of the method of forming the gel body when drying the gel body by hanging it in the air according to the present invention, and Figure 5 shows the load on the dry gel during sintering according to the present invention. An explanatory diagram of how to hang it. 11... Type having a glass disk shape with groups Group pitch group Width group Height Glass disk group with groups Pitch group Width group Depth group Dry gel having a glass disk shape with groups 22... Alumina load 23... Alumina base 31... Wet gel having a glass disk shape with a group 32 ・ 33 ・ 4 l ・ 42 ・ 43 ・ 44 ・ 5 l ・ 52 ・ 53 ・ 54 ・ 55 ・ Support dry container hole support part gel hanging Lowering jig Load Dry gel base Pattern transferred area Pattern untransferred area Above Applicant Seiko Epson Co., Ltd. Agent Patent attorney Kizobe Suzuki (and 1 other person) / 44 (years) (b) 7th + day Figure 3 Figure 5

Claims (5)

[Claims] (1) Prepare a liquid sol with a desired glass component composition using one or more metal alkoxides as main raw materials, and gel the liquid sol while contacting a matrix having a desired shape or pattern to produce a wet gel. After that, the wet gel is vitrified by heat treatment such as drying and sintering. A method for producing fine pattern transfer glass by a sol-gel method, characterized in that the wet gel is dried under supercritical conditions. A method for manufacturing fine pattern transfer glass. (2) A method for producing fine pattern-transferred glass by a sol-gel method, characterized in that the wet gel is dried in a liquid. (3) A method for producing fine pattern-transferred glass using a sol-gel method, characterized in that the wet gel is suspended in the air and dried. (4) When sintering the dry gel obtained by drying the wet gel in the method for producing fine pattern transfer glass according to the first, second, or third item, a load is applied to the dry gel. A method for producing fine pattern-transferred glass, characterized by sintering it while following the shape of a base. (5) A liquid sol having the desired glass component composition to be used in the method for producing fine pattern transfer glass as described in item 1 or 2 or 3 or 4 is mixed with one or more metal alkoxides and A method for producing fine pattern-transferred glass, which is characterized by preparing fine pattern-transferred glass using metal oxide fine particles as a main raw material.