CN107140810B - Method for manufacturing optical glass with secondary clarification - Google Patents
Method for manufacturing optical glass with secondary clarification Download PDFInfo
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- CN107140810B CN107140810B CN201710288954.0A CN201710288954A CN107140810B CN 107140810 B CN107140810 B CN 107140810B CN 201710288954 A CN201710288954 A CN 201710288954A CN 107140810 B CN107140810 B CN 107140810B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/225—Refining
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
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- Glass Melting And Manufacturing (AREA)
Abstract
The invention belongs to the technical field of optical glass preparation, and particularly relates to a method for manufacturing optical glass through secondary clarification. The invention has simple process and low cost, the melting part has a primary clarification function besides the melting function, the glass liquid can be discharged cleanly after entering the clarification part for secondary clarification, the satisfactory clarification quality is obtained, the high-quality optical glass bubble standard is achieved (360mm 160mm 20mm glass has no more than 1 bubble with the diameter larger than 0.02mm visible to naked eyes under the detection of a 35W spotlight), and the optical uniformity of the optical glass can be improved.
Description
Technical Field
The invention belongs to the technical field of optical glass preparation, and particularly relates to a manufacturing method of optical glass with secondary clarification.
Background
Glass melting is a very complex process that involves a series of physicochemical reactions. The result of these reactions is a mechanical mixture of the various raw materials that becomes a chemically bonded homogeneous glass melt. Many defects such as bubbles, stones, striae, etc. are sometimes generated during the glass melting process, and these defects are the main factors affecting the quality of the glass.
The clarification process of the molten glass is mainly a process for eliminating visible bubbles, is an extremely important link in the glass melting process, and is closely related to the quality of glass products. During the silicate reaction and glass formation, large amounts of gas are generated by the decomposition of the batch materials, volatilization of certain components, redox reactions of the batch materials, interaction of the glass with gaseous media and with refractory materials, and the like. Most of the gas will escape from the molten glass and the remaining part will dissolve in the molten glass and reform compounds with some of its constituents. Thus, the gas present in the glass is mainly in three states, i.e., bubbles, dissolved gas, chemically bound gas.
With the development of glass melting technology, glass electric melting technology is widely applied to some special glass systems (such as borosilicate glass, aluminum silicon glass, low alkali glass fiber and electronic display glass) more and more than the traditional soda-lime glass.
At present, the melting part of the existing continuous melting kiln only has a melting function and is not designed with a primary clarifying function, the clarification of bubbles is completed by a clarifying part, the design size and temperature requirements of the clarifying part are relatively high, and the difficulty of removing bubbles in the clarifying part is high and the risk of influencing the internal quality of glass by container materials is increased when the glass with large viscosity is produced due to the enlargement of the size and the increase of the temperature of the clarifying part; or the melting part of the existing continuous melting kiln is designed with a clarification function, but the melting part and the clarification part are not obviously cut, the clarification is not sufficient (the material channel only has a cooling function), and the standard of high-quality glass bubbles is difficult to achieve (360X 160X 20 glass has no more than 1 bubble with the macroscopic diameter larger than 0.02 under the detection of a 35W spotlight); or the melting part of the existing continuous melting furnace is partially provided with a primary clarifying function, and a clarifying part for secondary clarification is also designed, but an ascending channel is designed between the melting part and the clarifying part, the ascending process of the molten glass is a cooling process, and no matter the platinum ascending channel or the AZS refractory ascending channel, in order to ensure the high temperature of the clarifying part for secondary clarification, the molten glass in the ascending channel needs to be heated, so that the failure rate of platinum or the corrosion of the refractory material is aggravated, particularly the later, the service life of the furnace is influenced, and the quality of the intrinsic bubble in the glass is adversely affected.
Disclosure of Invention
The invention aims to overcome the technical defects and provide a method for manufacturing secondary clarified optical glass, which has the advantages of low cost, thorough clarification, better internal quality of the optical glass and higher quality.
In order to achieve the technical purpose, the invention provides a manufacturing method of optical glass with secondary clarification, which comprises the steps of putting a glass raw material into a melting part, wherein at least 2 heating zones are vertically or horizontally arranged in the melting part in sequence, each heating zone is internally provided with an electrode, the glass raw material is preheated and melted by a first heating zone in the heating zones to form glass liquid, the temperature of the first heating zone is 1350-.
As a modification, the melting part and the clarifying part are distributed in a step shape, and the melting part is positioned above the clarifying part.
As an improvement, the platinum flow guide pipe is provided with 2-4 flow guide temperature control areas.
As an improvement, the platinum guide pipe is arranged at a position 100-200mm away from the bottom of the melting part.
As an improvement, the clarification part is provided with 2-3 clarification temperature control areas, and electrodes are arranged in the clarification temperature control areas.
As an improvement, the rear end of the clarification part is provided with a platinum communicating pipe, a platinum stirrer and a platinum homogenizing pool, the platinum stirrer is arranged in the platinum homogenizing pool, the platinum communicating pipe is communicated with the platinum homogenizing pool, and a liquid level monitoring hole is formed in the platinum communicating pipe.
As a further improvement, the platinum guide pipe is provided with a plurality of platinum guide branch pipes, and each platinum guide branch pipe is communicated with one clarification part.
As a further improvement, 3 heating zones are arranged in the melting part, a temperature measuring point is arranged in each heating zone, the electrodes are arranged on the side part or the bottom part of the melting part, a cover top is arranged at the top part of the melting part, a bubbler is arranged at the bottom part of the melting part, a kiln bank is arranged at the middle rear part of the melting part along the length direction, and electric boosting is arranged at the bottom part or the side part of the melting part.
As a further improvement, a powder layer is arranged on the upper part of the molten glass.
Preferably, the melting part is square, hexagonal or rectangular.
The invention has the beneficial effects that:
the invention provides a method for manufacturing optical glass with secondary clarification, which has simple process and low cost, wherein glass raw materials are heated and melted by a first heating zone to form molten glass, after the molten glass enters a second heating zone to reach the clarification temperature, partial clarifying agent in the glass raw materials releases oxygen, the oxygen can take bubbles in the molten glass away to achieve the purpose of primary clarification, a melting part has the function of primary clarification besides the melting function, the molten glass which is subjected to the primary clarification is guided into a clarification part by a platinum guide pipe, the service lives of the melting part and the clarification part can be prolonged, secondary clarification is carried out in the clarification part, bubbles in the molten glass can be discharged cleanly, satisfactory clarification quality is obtained, and the high-quality optical glass bubble standard (360mm 160mm 20mm glass is detected by 35W, bubbles with the diameter larger than 0.02mm are not more than 1 by naked eye), the optical uniformity of the optical glass can be improved.
Drawings
FIG. 1 is a side view of a melting section and a fining section of an embodiment of the present invention;
FIG. 2 is a top view of a melting section and a fining section of an embodiment of the present invention;
the device comprises a melting part 1, a capping part 2, a powder layer 3, a platinum guide tube 4, a clarification part 5, a liquid level monitoring hole 6, a platinum stirrer 7, a platinum homogenizing pool 8, a platinum communicating tube 9, an upper electrode 10, an upper electrode temperature measuring point 11, a middle electrode 12, a middle electrode 13, a middle electrode temperature measuring point 14, a lower electrode 15 and a carbon rod 16.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in FIG. 1, a method for manufacturing optical glass by secondary refining uses an apparatus comprising a melting section 1 and a refining section 5, wherein the melting section 1 and the refining section 5 are arranged in a stepped manner and are separated from each other, and molten glass is guided between the melting section 1 and the refining section 5 through a platinum flow guide tube 4. Preferably, the area of the melting part 1 is 6 square meters, and the depth is 2 meters; the length of the clarification section 5 is 6 meters (the front part is 750 meters wide and 4.2 meters long, the rear part is 950 meters wide and the length is 1.8 meters),
the top of the melting part 1 is provided with a cover top 2, 2-3 heating zones are arranged in the melting part 1, 3 heating zones are shown in fig. 1, namely a first heating zone, a second heating zone and a third heating zone, each heating zone is internally provided with an electrode and a temperature measuring point, the first heating zone, the second heating zone and the third heating zone are respectively and correspondingly provided with an upper electrode 10, an upper electrode temperature measuring point 11, a middle electrode 12, a middle electrode temperature measuring point 13, a lower electrode 14 and a lower electrode temperature measuring point 15, the temperature of the first heating zone is preferably 1350-.
According to the requirements of different formulas, the electrodes can be selected from a molybdenum electrode, a tin electrode and a platinum electrode, the glass liquid is directly heated by using a two-phase or three-phase power supply by utilizing the principle of joule heat to reach the temperature of the glass liquid required by 2 to 3 heating areas of the melting part 1, so that the functions of preheating, melting and primarily clarifying the glass raw material are achieved; for K-type optical glass, a molybdenum electrode is preferred; for F type and environment-friendly F type phosphate glass optical glass, a tin electrode is selected; for optical glass with high quality and high transmittance, platinum electrode is preferred.
As shown in fig. 2, the shape of the melting portion 1 may be hexagonal, or may be other polygonal shapes such as square, rectangle, and the like. For the melting temperature below 1400 ℃, a tin electrode is preferred, a two-phase power supply mode is preferred, three heating zones are preferred along the height direction, and the electrode is preferred to be inserted laterally; for a hexagon or a polygon, molybdenum electrodes are firstly selected for heating, three-phase power supply and two-phase power supply can be selected, the electrodes can be selected to be inserted laterally or inserted bottom, and the electrodes are preferably selected to be inserted laterally; for soda-lime-silica glass, a square melting part can be selected, electrodes are preferentially inserted laterally, two-phase power supply is performed, tip conduction and lateral conduction modes can be selected, and lateral conduction modes are preferentially selected.
As shown in figure 1, the space between the cover top 2 and the molten glass can be heated, the heating mode can adopt a cold top mode, a flame heating mode, a carbon rod mode, a silicon-molybdenum rod mode and the like, the cold top mode is preferred for a melting part which is vertically melted, namely, the upper part of the molten glass is provided with a powder layer 3, the glass raw material is directly used as an electric conductor of Joule heat effect after being melted into the molten glass at high temperature, the melting is realized by the self electric conduction of the molten glass, the liquid surface of the glass is covered by a layer of powder, the temperature of the upper space is only 70-150 ℃, because the heat generated by the electric conduction of the molten glass is absorbed by the glass, the hot gas carries a small amount of heat energy and the heat on the outer surface of the melting part is dissipated during charging, the; flame heating is preferred for horizontally melting sections.
The bottom or the side part of the melting part 1 is provided with electric boosting, and a molybdenum electrode is preferred for soda-lime-silica, microcrystalline glass and high borosilicate; the tin electrode is selected for special glass; either a two-phase or a three-phase power supply may be selected. A bubbler can be arranged along the width direction of the melting part 1, is generally arranged at the bottom of the melting part, and can change the flow stroke of the glass liquid and increase the melting time; and a kiln bank is arranged at the middle and rear section of the length of the melting part 1 to change the thickness of the molten glass and enhance the clarification of the molten glass.
The position which is 200mm away from the bottom of the melting part 1 is provided with a platinum draft tube 4, the position which is 150mm away from the bottom is preferably provided with the platinum draft tube 4, the platinum draft tube 4 is directly electrified to heat the glass liquid, 2 to 4 flow guide temperature control regions are generally arranged, and 4 flow guide temperature control regions (MF1, MF2, MF3 and MF 4) are preferably selected, wherein the flow guide temperature control regions can ensure the stable flow of the glass liquid flowing into the clarification part and the required glass viscosity of the clarification part, the platinum draft tube 4 ensures the required high temperature of the clarification part, the temperature of the glass liquid in the process that the melting part 1 flows into the clarification part 5 cannot be reduced, the sufficient heat supply needs to be provided for the clarification part, and the diameter of the platinum draft tube 4 is calculated according to the viscosity, the flow and the position drop of the glass liquid in the clarification part 5 to ensure that. The platinum flow guide pipe 4 can be designed into a form that one main pipe is divided into a plurality of platinum flow guide branch pipes, the number of the branch pipes is determined according to the number of clarification parts (production lines), 1 to 3 clarification parts (or production lines) are preferentially selected, and the diversified requirements of one optical glass brand and different products are realized.
According to different formulas of the glass, the material channel heating of the clarifying part 5 can select a molybdenum electrode, a tin electrode, a carbon rod 16 and natural gas to heat independently, and also can select the combination of the molybdenum electrode and the carbon rod 16 or the natural gas, or the combination of the tin electrode and the carbon rod 16 or the natural gas, so that the viscosity of the glass in the clarifying part can meet the process requirement. For the formulation containing B2O3The fluoride of (2) is preferably heated by matching a molybdenum electrode or a tin electrode with natural gas; for soda-lime-silica glass, the heating mode of combining the molybdenum electrode and the carbon rod 16 is preferably selected;for lead-containing glass and high-barium and high-titanium glass, a heating mode of combining a tin electrode and the carbon rod 16 is preferably selected; for high alkali content and B2O3The silicate glass selects a molybdenum electrode independent heating mode preferentially; the tin electrode single heating mode is preferentially selected for phosphate glass, the platinum container is selected for a clarification part, and the carbon rod 16 is preferentially selected for space heating.
The clarification part 5 can select fused zirconia corundum bricks or platinum as a container material, high-quality fused zirconia corundum bricks are preferentially selected as the clarification part for optical glass such as soda-lime-silica, boron-containing silica and the like, and the elapsed time of molten glass is designed to be 4 to 6 hours, and is preferentially selected to be 6 hours when fused zirconia corundum is used as the container material; in the case where platinum is preferred as the vessel of the fluoride-and phosphate-containing glass and platinum is preferred as the vessel of the refining section 5, the elapsed time of the molten glass is designed to be 1 to 2 hours, preferably 1 hour.
As shown in figure 1, the rear end of the clarification part 5 is provided with a platinum communicating pipe 9, a liquid level monitoring hole 6 is formed in the platinum communicating pipe 9, a liquid level detector is installed above the liquid level monitoring hole 6 and detects that the liquid level is fed back to an electrode current control part of a platinum flow guide pipe 4, and the electrode current is increased or reduced according to the height of the liquid level to realize the stable control of the liquid level of the clarification part.
The platinum communicating pipe 9 is communicated with a platinum homogenizing pool 8, a platinum stirring tank 7 is arranged in the platinum homogenizing pool, and the platinum stirring tank 7 and the platinum homogenizing pool 8 are used for eliminating the internal stripes of the glass.
Method for manufacturing secondary clarified 10TK51 optical glass
Glass raw materials (mass percent): 270-72% of SiO, Na2O:11.5%~12.5%,K2O:8%~9.5%,B2O3:1.5%,CaO:8%~9%,BaO:1%~2%,TiO2:1%~2%,Sb2O30.1 to 1 percent. Refractive index: 1.52307 density: 2.53 g/cc; the melting temperature of the glass is 1350-1400 ℃; the fining temperature of the molten glass is 1450 ℃.
Setting parameters:
upper electrode voltage current: 105V/1300A temperature: 1350 degrees;
middle electrode voltage current: temperature of 110V/1420A: 1450 degrees;
lower electrode voltage current: 75V/400A temperature: 1350 degrees;
temperature of the platinum flow guide tube: MF 1: 1350 degree MF 2: 1360 degree MF 3: 1380 degree MF 4: 1400 degrees;
a clarification section: front end temperature CF 1: 1400 degrees; middle temperature CF 2: 1450 degrees; rear-stage temperature CF 3: 1400 degrees;
carbon rod power of clarification part: 80 KVA;
power of four molybdenum electrodes: 40 KVA;
space temperature of platinum homogenizing tank: 1200 to 1250 degrees;
liquid level of the clarification tank: the liquid level line is 230mm from the bottom;
continuously feeding materials by using an automatic feeder, wherein the powder in the melting tank is separated from the upper edge of the melting part by 100 mm;
rotation speed of platinum stirrer: 30 revolutions per minute;
the manufacturing process comprises the following steps:
the glass raw materials are put into a melting part, the glass raw materials are preheated and melted by the melting part to form molten glass, the residence time of the molten glass in the melting part is 48-60 hours, preferably 60 hours, the molten glass is preliminarily clarified by the melting part and then flows into a clarifying part through a platinum guide pipe for secondary clarification, the residence time of the molten glass in the clarifying part is 1-6 hours, the elapsed time of the molten glass is designed to be 4-6 hours when the clarifying part is an electric smelting zirconia corundum material, preferably 6 hours, and the elapsed time of the molten glass is designed to be 1-2 hours, preferably 1 hour when the clarifying part is a platinum material.
The product quality condition is as follows: the number of bubbles with the diameter larger than 0.02mm which can be seen by naked eyes under the detection of a 35W spotlight with 360mm 160mm 20mm glass accounts for 98 percent of the total number.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. The manufacturing method of the optical glass with the secondary clarification is characterized in that a glass raw material is put into a melting part, 3 heating zones are vertically and sequentially arranged in the melting part, the temperature of the first heating zone is 1350-, and the molten glass is primarily clarified by the second heating zone in the heating zones, after the molten glass enters the second heating zone and reaches the clarification temperature, part of clarifying agents in the glass raw materials release oxygen, the oxygen can take away bubbles in the molten glass, the purpose of primary clarification is achieved, the residence time of the molten glass in the melting part is 48-60 hours, the molten glass finally flows into the clarifying part through a platinum guide pipe to be secondarily clarified, and the residence time of the molten glass in the clarifying part is 1-6 hours.
2. The method of claim 1, wherein the melting section and the fining section are in a stepped configuration, and the melting section is located above the fining section.
3. The method for manufacturing optical glass for secondary clarification according to claim 1, wherein the platinum flow guide pipe is provided with 2-4 flow guide temperature control areas.
4. The method as claimed in claim 1, wherein the platinum guide tube is disposed at a distance of 100-200mm from the bottom of the melting section.
5. The method for manufacturing optical glass by secondary clarification according to claim 1, wherein the clarification part is provided with 2-3 clarification temperature control areas, and electrodes are arranged in the clarification temperature control areas.
6. The method for manufacturing optical glass by secondary clarification according to claim 1, wherein a platinum communicating pipe, a platinum stirrer and a platinum homogenizing pool are arranged at the rear end of the clarification part, the platinum stirrer is arranged in the platinum homogenizing pool, the platinum communicating pipe is communicated with the platinum homogenizing pool, and a liquid level monitoring hole is arranged on the platinum communicating pipe.
7. The method for producing optical glass by secondary refining according to any of claims 1 to 6, wherein the platinum flow guide pipe is provided with a plurality of platinum flow guide branch pipes, and each of the platinum flow guide branch pipes is communicated with one refining section.
8. The method of manufacturing double-fined optical glass according to claim 1, wherein the melting section is square, hexagonal or rectangular.
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CN111204955A (en) * | 2020-01-16 | 2020-05-29 | 成都光明光电股份有限公司 | Method for producing optical glass |
CN115367999A (en) * | 2022-09-21 | 2022-11-22 | 成都光明光电股份有限公司 | Intermittent optical glass production method and device |
Citations (2)
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US4932035A (en) * | 1987-05-30 | 1990-06-05 | Sorg Gmbh & Co. Kg | Discontinuous glass melting furnace |
US6085551A (en) * | 1997-03-14 | 2000-07-11 | Beteiligungen Sorg Gmbh & Co. Kg | Method and apparatus for manufacturing high melting point glasses with volatile components |
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CN201777972U (en) * | 2010-03-30 | 2011-03-30 | 湖北新华光信息材料股份有限公司 | Detachable optical glass continuous smelting furnace |
CN201842758U (en) * | 2010-08-19 | 2011-05-25 | 湖北戈碧迦光电科技股份有限公司 | Glass electric melting kiln |
CN103332850B (en) * | 2013-06-03 | 2015-12-16 | 湖北戈碧迦光电科技股份有限公司 | A kind of optical glass production line |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US4932035A (en) * | 1987-05-30 | 1990-06-05 | Sorg Gmbh & Co. Kg | Discontinuous glass melting furnace |
US6085551A (en) * | 1997-03-14 | 2000-07-11 | Beteiligungen Sorg Gmbh & Co. Kg | Method and apparatus for manufacturing high melting point glasses with volatile components |
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