CN104402197A - Low water content quartz glass material preparation method - Google Patents
Low water content quartz glass material preparation method Download PDFInfo
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- CN104402197A CN104402197A CN201410574097.7A CN201410574097A CN104402197A CN 104402197 A CN104402197 A CN 104402197A CN 201410574097 A CN201410574097 A CN 201410574097A CN 104402197 A CN104402197 A CN 104402197A
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- quartz glass
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- material preparation
- glass material
- water content
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Abstract
A low water content quartz glass material preparation method belongs to the field of material preparation. In view of the problem that glass samples prepared by a preparation method in the prior art has long hydroxyl (OH group), the glass material preparation method capable of removing most of the hydroxyl is provided. According to the preparation method, tetraethoxysilane, ethanol and formamide are mixed according to the volume ratio of 2:3:1, and 0.04mol / L dilute hydrochloric acid is added into the mixed liquor, so that the molar ratio of water molecules to tetraethoxysilane molecules reaches 10:1, sol is produced by fully stirring, then the produced sol is put into a polytetrafluoroethylene die, and dried into gel at 40 DEG C; and the dry gel sample is burnt to 1200 DEG C by strictly controlled heating process (1 DEG C / min), and cooled for formation of a pure quartz glass sample. The quartz glass material prepared by the method basically can completely remove the residual hydroxyl groups, and can be used as excellent optical materials.
Description
Technical field
The invention belongs to glass material preparation field.
Background technology
Silica glass is irreplaceable optical material in semiconductor material photoetching technique, sol-gel method is a kind of method that conventional chemical means prepares glass material, the method preparing glass material with other is compared, have the advantages that technique is simple, cost is low and can prepare at a lower temperature, but preparation 157nm high permeability silica glass, existence thoroughly will remove hydroxyl (OH group) long in sample, because OH group can affect the absorption of material at below 180nm to a great extent.
Summary of the invention
The object of this invention is to provide a kind of method can preparing the quartz glass body material of low OH content.
The present invention is achieved by the following technical programs: a kind of low water content quartz glass body material preparation method, by tetraethoxy, ethanol and methane amide mix according to the ratio of volume ratio 2:3:1, the dilute hydrochloric acid of 0.04mol/L is added in mixed solution, the mol ratio of water molecules and tetraethoxy molecule is made to reach 10:1, and fully stir, after colloidal sol generates, put into the mould of tetrafluoroethylene, dry formation gel at 40 DEG C; Xerogel sample passes through strict temperature-rise period (1 DEG C/min) calcination always controlled to 1200 DEG C, the pure quartz glass samples of formation after cooling.
By oxygen, tetracol phenixin is brought in described calcination process, around sample, form O
2/ CCl
4atmosphere.
Described calcination process is carried out in temperature control quartz stove.
The present invention has following beneficial effect:
The present invention adopts sol-gel technique, by specific chemical seasoning method.Obtain the vitreum material of low OH content.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Specific embodiment: the method for the invention: by tetraethoxy, ethanol and methane amide mix according to the ratio of volume ratio 2:3:1, the dilute hydrochloric acid of 0.04mol/L is added in mixed solution, the mol ratio of water molecules and tetraethoxy molecule is made to reach 10:1, and fully stir, methane amide here uses as drying control agent.The mould of tetrafluoroethylene is put into after colloidal sol generates, dry formation gel at 40 DEG C, tetracol phenixin to 1200 DEG C through strict temperature-rise period (1 DEG C/min) calcination always controlled, is brought into by oxygen in calcination process, around sample, is formed O by xerogel sample in temperature control quartz stove
2/ CCl
4atmosphere, because xerogel is vesicular structure on microcosmic, utilizes the chemical reaction of residual hydroxy groups in tetracol phenixin and sample space can reach the object thoroughly removing hydroxyl, forms pure quartz glass samples after calcination cooling.
By glass sample through surface finish and polishing, survey its infrared absorption line, calculate the OH group content in glass sample is lowered to 2.8 × 10
-4, can use as the glass that optical quality is good.
Preparation method described in the embodiment of the present invention, can obtain the silica glass of low OH group, can use as excellent optical material.
above content is the further description done the present invention in conjunction with concrete embodiment, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (3)
1. a low water content quartz glass body material preparation method, it is characterized in that: by tetraethoxy, ethanol and methane amide mix according to the ratio of volume ratio 2:3:1, the dilute hydrochloric acid of 0.04mol/L is added in mixed solution, the mol ratio of water molecules and tetraethoxy molecule is made to reach 10:1, and fully stir, after colloidal sol generates, put into the mould of tetrafluoroethylene, dry formation gel at 40 DEG C; Xerogel sample passes through strict temperature-rise period (1 DEG C/min) calcination always controlled to 1200 DEG C, the pure quartz glass samples of formation after cooling.
2. preparation method as claimed in claim 1, be is characterized in that: brought into by tetracol phenixin by oxygen in described calcination process, around sample, form O
2/ CCl
4atmosphere.
3. preparation method as claimed in claim 1 or 2, is characterized in that: described calcination process is carried out in temperature control quartz stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410574097.7A CN104402197A (en) | 2014-10-24 | 2014-10-24 | Low water content quartz glass material preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410574097.7A CN104402197A (en) | 2014-10-24 | 2014-10-24 | Low water content quartz glass material preparation method |
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| CN104402197A true CN104402197A (en) | 2015-03-11 |
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ID=52639884
Family Applications (1)
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|---|---|---|---|
| CN201410574097.7A Pending CN104402197A (en) | 2014-10-24 | 2014-10-24 | Low water content quartz glass material preparation method |
Country Status (1)
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330134A (en) * | 2015-12-04 | 2016-02-17 | 太仓市建兴石英玻璃厂 | Preparing method for fluorine-high-doped silica glass |
| CN108698888A (en) * | 2015-12-18 | 2018-10-23 | 贺利氏石英玻璃有限两合公司 | Preparation in quartz glass preparation as the silica dioxide granule through carbon doping of intermediary |
| US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
| US11708290B2 (en) | 2015-12-18 | 2023-07-25 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
-
2014
- 2014-10-24 CN CN201410574097.7A patent/CN104402197A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330134A (en) * | 2015-12-04 | 2016-02-17 | 太仓市建兴石英玻璃厂 | Preparing method for fluorine-high-doped silica glass |
| CN108698888A (en) * | 2015-12-18 | 2018-10-23 | 贺利氏石英玻璃有限两合公司 | Preparation in quartz glass preparation as the silica dioxide granule through carbon doping of intermediary |
| US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
| US11339076B2 (en) | 2015-12-18 | 2022-05-24 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of carbon-doped silicon dioxide granulate as an intermediate in the preparation of quartz glass |
| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
| US11708290B2 (en) | 2015-12-18 | 2023-07-25 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150311 |
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| WD01 | Invention patent application deemed withdrawn after publication |