JPS6291428A - Production of glass - Google Patents

Abstract

PURPOSE:To prevent a foreign material such as refuse from mixing with glass and to enable the production of high-quality glass contg. less inner foreign material in a producing method of glass due to a sol-gel process by performing the preparation of sol in the clean atmosphere. CONSTITUTION:In such case that glass is produced by a sol-gel process, (A) the preparation of sol is performed in the clean atmosphere and (B) the preparation of sol is performed in the inside of a clean room cleaner than class 10000 and (C) during the preparing processes of sol, the process after a separation process removing a foreign material (refuse, a coarse silica grain and etc.) from sol is performed in the inside of the clean room cleaner than class 1000 and (D) a process charging the prepared sol in a desirably shaped vessel is performed in the atmosphere cleaner than class 100. Wherein 'class' is shown in >=0.5mump concn. (piece/ft<2>) of a floated grain. In such a way, remarkably high-quality glass contg. less inner foreign material is obtained by preparing sol in a clean atmosphere.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing glass by a sol-gel method.

[Summary of the invention]

The present invention is a method for producing glass using the sol-gel method. By preparing the sol in a clean atmosphere, the incorporation of foreign substances such as dust into the sol is prevented, and extremely high quality glass with few internal foreign substances is produced. This makes it possible to manufacture glass.

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[Conventional technology]

In glass production by the sol-gel method, the cleanliness of the atmosphere in which the sol is prepared has not been particularly controlled.

[Problems and Objectives to be Solved by the Invention] However, the above-mentioned prior art does not ensure the cleanliness of the atmosphere in which the sol is prepared. etc.) are mixed into the sol and remain in the manufactured glass.

Also, when preparing the sol, the cleanliness in the room is not constant, so 19.
Chamber':,lF2- There is a problem that the number of foreign substances in the glass produced varies (2) It is difficult to manufacture glass with stable purchase.

The present invention is intended to solve these problems, and its purpose is to make it possible to stably produce high-quality glass by controlling the cleanliness of the room during sol preparation, which was lacking in the conventional technology. An object of the present invention is to provide a method for manufacturing glass using a sol-gel method.

[Means for solving problems]

The method of the present invention is a glass manufacturing method characterized by performing sol preparation in a clean atmosphere in glass manufacturing by a sol-gel method.

[Effect]

According to the present invention, since there is almost no foreign matter (dirt, dust, etc.) mixed in from the outside during sol preparation, foreign matter is also present inside the glass obtained by gelling, drying, and sintering the sol. High-quality glass can be manufactured without the need for In addition, sosol xm using alkyl zorecate as the main raw material is At, T I,
Na, Ca, G.

By adding such as to the sol, it is easy to produce various multi-component glasses with straight sieve crystals.

〔Example〕

1) Polymer number ethyl/licade 28 (Si(OEt)4
) 162tα01NHae108t and ultrafine particle glue force (1 product name: Ae Uji oxso (Degussa)) 4
Mix 5 and 7 at the same time and stir for 4 hours using a disilver (stirring and dispersing device) to obtain ethylsilic.
At the same time, a sol containing a certain fraction of ultrafine silica particles was prepared, and in order to further improve its external resistance, the sol was subjected to ultrasonic irradiation (combined with stirring) for 5 hours. At this time, in order to prevent the sol temperature from increasing due to the supercalf wave irradiation, the sol temperature was kept constant using a cooling device [d].

As the next step, the sol is centrifuged (3000 rpm) to remove semi-gelled jelly-like substances, large particles containing impurities, and dust.

10-30 rlin) was added. After this, the sol was further filtered to remove foreign substances. Then, while stirring the sol, add CLIN ammonia water.
-' 4- After adjusting the pH value to 3 to 6 and pressing for 20 minutes, centrifugation was performed for 111 minutes to remove gel particles generated at this time.
(30[11[]]rpII+, 10-10-5O),
After undergoing re-offing treatment, the size is 36 x 24 x 12 [11n].
A total of 400 containers, each at 600 F, were placed in polypropylene containers and gelatinized in a sealed state. After that, when the shrinkage starts, change the lid of the container to one with a predetermined porosity with holes to adjust the drying speed, put it in a dryer, and heat it from room temperature at a heating rate of 5 C/hr to 60~60 hr. Heat it to 80℃ and keep it at this temperature for 10 to 15 days until it grows to 2.
5±(L5)X(15±α5)×(α5±0.2)(
- dry gel was obtained.

These dried gels were placed in a sintering furnace and heated and sintered using a predetermined heating method to form a transparent glass body at 1300 to 1450C. The size of this glass is (18±α5)×(1
1±[L5)X(α6±0.05)
It was 0±5 [t].

When the hemorrhoidal glass was observed using an optical microscope or a condensing lamp, it was found that there was a foreign object (size O ~
200 μm), and their number varied considerably depending on the valley glass.

In addition, the results of various physical property analyzes regarding these glasses were completely consistent with those of the fused stone Kengaranu, including Vickers hardness, fossilization, coefficient of thermal expansion, infrared absorption spectrum, near-infrared absorption spectrum, and refractive index.

In this case, the sol preparation process did not control the cleanliness of the room at all.

2) Silica glass was manufactured in exactly the same manner as in Example 1. However, here, the entire sol preparation process was performed in a class 10,000 clean room. The glass obtained at this time was observed using an optical microscope, condensing lamp, etc. in the same manner as in Example 1. Although there were foreign substances in the glass, compared to Example 1, the number of foreign substances and the variation among each glass were found. has become very small.

3) Silica glass was produced in exactly the same manner as in Example 1. However, in this case, the steps in the sol preparation process from centrifugation to input into eight vessels were performed in a class 800 clean room. When the glass obtained at this time was observed using an optical microscope and a condensing lamp in the same manner as in Example 1, it was found that the number of foreign substances and the variation among each glass were smaller than in Example 2. Ta.

4) Silica glass was produced in the same manner as in Examples 1 to 6, except that the entire process from final filtration of the prepared sol to charging into a container was carried out in a class 0 to 100 clean atmosphere. When the glasses obtained at this time were similarly inspected using an optical microscope and a condensing lamp, there were almost no foreign substances in each glass. A comparison of the number of foreign objects is shown.

Table 1. Comparison of proboscis within the glass [Effect of the invention] As described above, the six-key glass manufactured by the present invention is manufactured in a clean atmosphere, so there is no contamination of foreign matter from the outside, and therefore the glass It will be of high quality with no foreign substances inside. Moreover, unlike the conventional method, there is almost no variation between products, and it is possible to manufacture high-quality 6-key glass at a high yield.

As mentioned above, in addition to having advantages such as low cost compared to the fusion method, very high quality quartz glass can be easily manufactured and used in fields where quartz glass has been used up until now. Of course, it has wide applications in many fields such as RC photomask substrates and optical fiber base materials.
think of it as something that Also, ^l.

Reciting elements such as TI, Go, Na, Mg, Ll, Tea, etc.
By adding it during the production of Sol fA, it is also possible to produce a multi-component glass of high quality.

that's all

Claims (1)

[Claims] (1) A method for producing glass by the sol-gel method, characterized in that the following conditions are met during the sol preparation process. a) Perform the sol preparation in a clean atmosphere b) Perform the sol preparation in a clean room that is cleaner than class 10,000 c) During the sol preparation process, after the step of separating foreign substances (dust, coarse silica particles, etc.) from the sol d) The step of charging the prepared sol into a container of the desired shape is carried out in a clean room that is cleaner than Class 1,000 (however, "class" refers to the concentration of suspended particles of 0.5 μmp or higher). Represents [pieces/ft^3].)