WO2010001857A1 - Procédé de fabrication d'un corps formé de verre et dispositif de fabrication - Google Patents

Procédé de fabrication d'un corps formé de verre et dispositif de fabrication Download PDF

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Publication number
WO2010001857A1
WO2010001857A1 PCT/JP2009/061851 JP2009061851W WO2010001857A1 WO 2010001857 A1 WO2010001857 A1 WO 2010001857A1 JP 2009061851 W JP2009061851 W JP 2009061851W WO 2010001857 A1 WO2010001857 A1 WO 2010001857A1
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Prior art keywords
melt
manufacturing
electrodes
dissolution tank
glass
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PCT/JP2009/061851
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English (en)
Japanese (ja)
Inventor
孝之 岸
直雪 後藤
稔 梅田
直人 佐藤
寛 岡野
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株式会社オハラ
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Priority to CN200980124596.3A priority Critical patent/CN102076619B/zh
Publication of WO2010001857A1 publication Critical patent/WO2010001857A1/fr

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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
    • C03B5/02—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating
    • C03B5/027—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating by passing an electric current between electrodes immersed in the glass bath, i.e. by direct resistance heating
    • C03B5/0275—Shaft furnaces
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B3/00—Charging the melting furnaces
    • 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
    • C03B5/18—Stirring devices; Homogenisation
    • C03B5/187—Stirring devices; Homogenisation with moving elements
    • 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
    • C03B5/235—Heating the glass
    • 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
    • C03B5/42—Details of construction of furnace walls, e.g. to prevent corrosion; Use of materials for furnace walls
    • C03B5/43—Use of materials for furnace walls, e.g. fire-bricks

Definitions

  • the present invention relates to a method for manufacturing a glass molded body and a manufacturing apparatus.
  • a melting apparatus for continuously obtaining glass a melting tank, a clarification tank, and a stirring tank are sequentially provided, and the raw material is replenished so that the level of the melt is always substantially constant.
  • a continuous melting furnace is often used in which the melted liquid is sequentially moved to a clarification tank and a stirring tank.
  • Patent Document 1 discloses a batch-type melting furnace (a melting furnace that stops the replenishment of raw materials when a certain amount of melt is obtained while stopping the outflow of glass, and then starts outflow of glass). A technique for forming a large-capacity glass block using the same is disclosed.
  • the present invention has been made in view of the above circumstances, and provides a method and apparatus for manufacturing a glass molded body that can cope with the molding of a large volume glass block and can sufficiently improve the homogeneity of the glass.
  • the large-volume glass block refers to, for example, a block having a size of 0.3 m 3 or more.
  • glass contains the crystallized glass which heat-processed and crystallized amorphous glass and amorphous glass.
  • the present inventors heated the melt from above the melt while energizing and heating the melt, and inserting and removing the stirrer at an appropriate timing, so that the temperature of the melt is appropriately controlled,
  • the inventors have found that the melt can be sufficiently stirred while suppressing damage, and have completed the present invention.
  • the present invention provides the following.
  • the temperature of the melt in a range of 1 ⁇ 4 or less of the melt depth from the bottom of the dissolution tank is set to 1 ⁇ 4 or less of the melt depth from the liquid surface.
  • the manufacturing method as described in (1) which has a temperature difference setting process made higher than the temperature of the melt in the range.
  • the plurality of electrodes one having a cooling mechanism inside and projecting substantially inward into the dissolution tank is used, and the plurality of electrodes are cooled by the cooling mechanism (1) to (3 ) Any one of the manufacturing methods.
  • a part or all of the upper furnace wall and / or the lower furnace wall in which the melt is accommodated as the melting tank is selected from the group consisting of an electroformed refractory, a refractory brick, and a ceramic fiber.
  • a flue having an adjustable opening is provided on the upper furnace wall, and the opening of the flue is adjusted so that the internal pressure of the melting tank falls within a predetermined range.
  • the manufacturing method in any one of (11).
  • the ratio (a / b) of the combustion amount a (kcal / h) per unit time of the combustion burner to the raw material supply amount b (L) is set to 400 or less (1) to (14) Manufacturing method.
  • An apparatus for manufacturing a glass molded body A dissolution vessel having a plurality of electrodes in which a raw material melt is contained and immersed in the melt; A feeder communicating with the dissolution tank; Heating means provided in the upper part of the dissolution tank; A mold for molding molten glass derived from the feeder; A stirring device that can be inserted into and removed from the inside of the dissolution tank.
  • the stirrer has a refrigerant flow path therein, high expansion ceramics is provided around the refrigerant flow path, and the high expansion ceramic is coated with platinum or a platinum rhodium alloy (24 ) Manufacturing apparatus described.
  • the melting tank has a lower furnace wall for storing the melt, and an upper furnace wall provided on the upper part of the lower furnace wall,
  • the said heating means is a manufacturing apparatus in any one of (24) to (27) which has a combustion burner provided in the said upper furnace wall.
  • the melt is heated by the plurality of electrodes and is also heated from above, so that the raw materials are rapidly dissolved. Moreover, since the lower part of the melt is heated by energization heating, the convection of the melt is promoted, and clarification and homogenization are also quickly performed. And since a stirring body is inserted after fuse
  • FIG. 1 is a vertical sectional view of a glass molded body manufacturing apparatus 10 according to an embodiment of the present invention.
  • FIG. 2 is a plan view of the manufacturing apparatus 10 before the raw material is charged (however, the upper wall 263 of the upper furnace wall 26 is seen through).
  • the manufacturing apparatus 10 includes a dissolution tank 20, a feeder 30, a heating unit 40 as a heating unit, a mold 50, and a stirring body 60. Each component will be described in detail below.
  • the melting tank 20 contains a raw material melt.
  • the raw material may be a batch (a mixture of raw material powders of each component) or a rough melt cullet that is vitrified, and is placed on a holding unit 73 provided at the front end of the main body 71 of the raw material supply unit 70. , And supplied through a supply hole 237 formed in the side wall 231′a.
  • the supply hole 237 is formed so as to be openable and closable so that the temperature inside the dissolution tank 20 is not easily lowered, and is preferably opened when the raw material is supplied and closed during the rest.
  • the dissolution tank 20 has a plurality of electrodes 21a to 21d and 21′a to 21′d in the melt, and the plurality of electrodes 21a to 21d and 21′a to 21′d. Is electrically connected to a power source (not shown).
  • a power source not shown.
  • energization is performed through the melt and the melt is heated.
  • the temperature of the furnace and the melt are appropriately controlled in each step of melting, clarifying, and stirring the raw materials by heating by energization through the melt and heating from above of the melt by the heating unit 40 described later. Is possible.
  • the heating is performed only by the heating unit 40 until a certain amount of melt is obtained.
  • the electrodes 21a to 21d and 21'a to 21'd are installed in the lower part of the dissolution tank 20, the electrodes 21a to 21d and 21'a to 21a can be used when a certain amount of melt is stored.
  • the degree of current heating by 21'd and relatively weakening the heating from above the melt the temperature of the lower part of the melt becomes higher than the upper part. As a result, convection of the melt is promoted, and dissolution and clarification are rapidly performed.
  • the melt temperature in the range of 1 ⁇ 4 or less of the melt depth from the bottom 233 of the dissolution tank 20 can be changed from the melt surface FL to the melt depth in that a strong melt convection can be easily obtained. It is preferable to make it higher than the temperature of the melt in a range of 1 ⁇ 4 or less.
  • This temperature difference is caused by the temperature sensors 22a to 22c provided inside the lower furnace wall 23 containing the melt and the temperature sensors (not shown) provided inside the electrodes 21a to 21d or 21'a to 21'd. May be performed by adjusting the current heating by the electrodes 21a to 21d or 21'a to 21'd and the degree of heating by the heating unit 40, which will be described later, on the basis of the melt temperature of each part detected in (1).
  • the temperature difference may be set as appropriate according to the viscosity of the melt, but is preferably 10 ° C. or higher.
  • the lower limit of the temperature difference is more preferably 25 ° C, and most preferably 40 ° C.
  • the temperature difference is preferably 150 ° C. or less, more preferably 130 ° C. or less, and most preferably 100 ° C. or less in order to suppress an increase in cost spent for energization and erosion of the furnace wall by the melt.
  • the temperature of the melt is measured as follows. That is, a temperature sensor such as a thermocouple coated with platinum is projected into the melt from a hole provided in the furnace wall, and measurement is performed by the temperature sensor. Alternatively, it may be measured by a temperature sensor provided on the inner side of the tip of the electrodes 21a to 21d projected into the melt.
  • the electrodes 21a to 21d and 21'a to 21'd have a cooling mechanism (not shown) inside and project substantially horizontally inward of the dissolution tank 20. Since the electrodes 21a to 21d and 21'a to 21'd are cooled by the cooling mechanism, deterioration due to a high-temperature melt can be suppressed.
  • the cooling mechanism may be a conventionally known one. Further, since the electrodes 21a to 21d and 21'a to 21'd project substantially horizontally inward of the dissolution tank 20, the temperature of the melt can be rapidly raised by energization.
  • the lower limit of the protruding length is preferably 20 mm, more preferably 50 mm, and most preferably 100 mm from the viewpoint that the temperature rise of the melt can be made efficient.
  • the upper limit of the protruding length is preferably 700 mm, more preferably 600 mm, and most preferably 450 mm so that the amount of platinum or a platinum rhodium alloy that erodes into the melt when energized is minimized.
  • the electrodes 21a to 21d and 21'a to 21'd are arranged to face each other as shown in FIG. 2, and are a pair of electrodes 21a and 21'a, a pair of electrodes 21b and 21'b, and an electrode 21c and 21 Energization is performed between the pair of 'c and the pair of electrodes 21d and 21'd (the number of electrodes is eight).
  • the ratio (b / c) of the feed amount b (L) of the raw material to the number c of the plurality of electrodes is 350 or less in that homogenization of the melt by convection of the melt can be promoted.
  • the upper limit of b / c is more preferably 325, and most preferably 300. Further, the lower limit of b / c is preferably 50, more preferably 65, and most preferably 75 in consideration of the installation cost of the electrode and the homogenization of the melt by convection.
  • the horizontal cross section inside the dissolution tank 20 at least at the electrode installation position is an n-square (n is an integer of 4 or more). And it is preferably an integer of 5 or more. That is, as shown in FIG. 5C, a horizontal cross section where n is 4 may be used, but in this case, there may be a place where current heating is relatively insufficient, such as a place surrounded by a dotted line.
  • n is preferably 5 or more, and most preferably 6 or more, such a portion is reduced. In the present embodiment, as shown in FIG.
  • the entire lower furnace wall 23 has an n-gonal horizontal section from the viewpoint of simplifying the configuration, but at least the internal horizontal section at the electrode installation position is an n-square shape. If it is. In order to make the heating of the melt in the plane direction uniform, it is more preferable that at least the internal horizontal cross section at the electrode installation position is a regular n-gon.
  • the horizontal cross section is a regular octagon.
  • the present invention is not limited to this.
  • the side walls 231a to 231c and 231′a to 231′c are smoothly curved surfaces 232a to 232h. (That is, there is no corner), and the horizontal cross section may be a circle (for example, a perfect circle or an ellipse) as shown in FIG. 5B, that is, n may be infinite.
  • the portions where the electrodes 21a to 21d and 21'a to 21'd are installed are flat surfaces as shown in FIG.
  • the power source connected to the electrodes 21a to 21d and 21'a to 21'd is not particularly limited, but is an AC power source having a frequency of 2.5 kHz or more in terms of improving the heating efficiency of the melt. preferable.
  • the dissolution tank 20 is provided with a liquid level detector 80. Based on the height value of the liquid level FL of the melt detected by the liquid level detector 80, the amount of supply of raw materials and / or derivation of the melt is determined. It is preferable to adjust. That is, when the detected value of the height of the liquid level FL falls within a predetermined range, the supply of the raw material is stopped, and the glass can flow out from a feeder 30 described later. When the detected value falls below the predetermined range, the supply of the raw material is performed. The raw material is supplied by the unit 70. Thereby, the quality of the glass can be stabilized, and deterioration due to the electrodes 21a to 21d and 21'a to 21'd being exposed to gas can be prevented.
  • the liquid level detector 80 in the present embodiment is a device that emits near infrared rays from the semiconductor laser toward the liquid level FL and detects the reflected light, but is not limited thereto.
  • h / H is 0.1 to 0. Adjust the feed rate of raw materials to be .6.
  • the relative positions of the electrodes 21a to 21d at the melt depth can be set to positions where effective convection of the melt can be obtained. If the liquid level becomes too high, the effect of heating by energization becomes insufficient, so the lower limit of h / H is more preferably 0.2, and most preferably 0.3.
  • the upper limit of h / H is more preferably 0.55, and most preferably 0.52.
  • the heating unit 40 is provided in the upper part of the dissolution tank 20 and heats the melt from above the melt. As a result, the temperature is raised not only at the bottom but also at the top of the melt, so that it is possible to control the temperature of the melt in the vertical direction in combination with the current heating by the electrodes. is there.
  • the heating unit 40 preferably has combustion burners 41a and 41b in terms of excellent temperature rise efficiency. These combustion burners 41a and 41b are provided in the upper furnace wall 26 located in the upper part of the lower furnace wall 23 which accommodates a melt.
  • the combustion burners 41a and 41b in the present embodiment are arranged to face each other from the side wall 261 of the upper furnace wall 26 inward. Air combustion, oxyfuel combustion, or the like can be used as the combustion burners 41a and 41b, but oxyfuel combustion is preferred from the viewpoint of enabling high-temperature dissolution.
  • the ratio (A: B) of the volume (A) above the liquid level FL in the dissolution tank 20 to the volume (B) of the melt is set to 1.0: 1.0 to 1.5: 1. It is preferably 0.
  • A: B is more preferably 1.0: 1.0 to 1.4: 1.0, and most preferably 1.1: 1.0 to 1.35: 1.0.
  • the “volume (A) above the liquid level FL in the dissolution tank” refers to the volume occupied by gas in the dissolution tank, and is usually a value obtained by subtracting the volume of the melt from the total volume of the dissolution tank 20. be equivalent to.
  • the adjustment of A: B is performed by increasing / decreasing the melt volume B through the supply of raw materials and / or the derived amount of the melt. You may go.
  • the liquid level FL it is preferable to set the liquid level FL so that the height difference ⁇ between the center position of the openings 43a and 43b of the combustion burners 41a and 41b and the liquid level FL is 300 mm or more. Accordingly, the openings 43a and 43b, which are generation sources of OH groups, are sufficiently separated from the melt, so that mixing of OH groups into the melt can be further suppressed.
  • the lower limit of the height difference ⁇ is more preferably 350 mm, and most preferably 400 mm.
  • the upper limit of the height difference ⁇ is preferably 850 mm, more preferably 700 mm, and most preferably 650 mm.
  • the liquid level FL may be set through the supply of raw materials and / or the amount of melt derived.
  • the combustion burners 41a and 41b are arranged so as to open in the horizontal direction or upward in the horizontal direction as in the present embodiment. If the combustion burner is opened downward from the horizontal direction, the flame is directed to the melt, so that there is an increased risk of mixing OH groups into the melt. However, according to the above configuration, such a risk is reduced. Therefore, mixing of OH groups into the melt can be further suppressed.
  • the upper furnace wall 26 in this embodiment has a shape in which the side wall 261 has a diameter larger than that of the side wall 231 of the lower furnace wall 23 for the same effect, and the openings 43a, 41a, 41b of the combustion burners 41a, 41b. Although 43b is hidden from the melt, it is not limited to such a configuration.
  • the ratio (a / b) of the combustion amount a (kcal / h) per unit time of the combustion burners 41a and 41b to the supply amount b (L) of the raw material is 400 in that mixing of OH groups into the melt can be further suppressed.
  • the following is preferable. If a / b is excessive, that is, if excessive combustion is performed with respect to the supply amount of the raw material to be heated, the amount of OH groups mixed into the melt per unit amount tends to increase.
  • the upper limit of a / b is more preferably 350, and most preferably 330.
  • the lower limit of a / b is preferably 50, more preferably 70, and most preferably 100. It is.
  • the combustion amount a (kcal / h) can be calculated based on the supply amount of gas (for example, oxygen gas or hydrocarbon gas) supplied to the combustion burners 41a and 41b.
  • the raw material supply amount b (L) is the volume (unit: liter) of the raw material supplied to obtain the amount of melt accommodated in the dissolution tank at that time.
  • the heating portion 40 the combustion burner 41a, was constructed in 41b is not limited thereto, MoSi 2 heating element (e.g. Kanthal Corp. of "Cantal Super") or SiC heating elements (e.g. Tokaikonetsukogyo Co. Elema heating element) or the like.
  • MoSi 2 heating element e.g. Kanthal Corp. of "Cantal Super”
  • SiC heating elements e.g. Tokaikonetsukogyo Co. Elema heating element
  • a part or all of the upper furnace wall 26 and / or the lower furnace wall 23 is formed of at least one selected from the group consisting of electroformed refractories, refractory bricks, and ceramic fibers. It is preferable. Thereby, deterioration of the upper furnace wall 26 due to a high temperature atmosphere generated by combustion in the combustion burners 41a and 41b and / or deterioration of the lower furnace wall 23 due to contact with a high temperature melt can be suppressed.
  • all of the lower furnace wall 23 and the upper furnace wall 26 are formed with one or more types selected from the group consisting of electroformed refractories, refractory bricks, and ceramic fibers. It is preferable that
  • Lower furnace wall 23 the portion in contact with at least melt the ZrO 2 as a main material, it is preferable to further comprising SiO 2 and / or Al 2 O 3.
  • the durability can be improved by using ZrO 2 as the main material, and the stability of ZrO 2 can be improved by using SiO 2 and / or Al 2 O 3 together, which greatly improves the erosion of the furnace wall by the melt. it can. This effect is particularly prominent in SiO 2 —Al 2 O 3 —Li 2 O glass.
  • the entire lower furnace wall 23 is formed of a material having substantially the same composition from the viewpoint of simplification of the configuration. However, it is only necessary that at least a portion in contact with the melt is formed of the material having the above composition. Further, depending on the situation, a portion where the glass liquid surface is easily eroded, particularly the melt FL portion, can be cooled from the outside to prevent erosion.
  • the upper furnace wall 26 of the melting tank 20 is provided with a flue 28 whose opening degree can be adjusted, and the opening degree of the flue 28 may be adjusted so that the internal pressure of the melting tank 20 falls within a predetermined range. preferable. Thereby, while being able to stabilize the quality of a glass molded object, since it is suppressed that OH group accumulate
  • the opening of the flue 28 is adjusted by the regulating valve, but is not limited to this.
  • the upper furnace wall 26 has a rectangular horizontal cross section, and the flue 28 is provided on one side of the side wall 261 where the combustion burners 41a and 41b are not provided.
  • An introduction pipe 29 is provided on the opposite side of the flue 28, and the introduction pipe 29 communicates the inside of the dissolution tank 20 with the outside air.
  • outside air is introduced into the dissolution tank 20 from the introduction pipe 29, and this outside air pushes the inside air of the dissolution tank 20 containing OH groups to the outside through the flue 28.
  • the flue 28 and / or the introduction pipe 29 are provided at the same height as or lower than the combustion burners 41a and 41b in that the OH group can be further prevented from being mixed into the melt.
  • the stirring body 60 is configured to be inserted into and removed from the inside of the dissolution tank. After the raw materials are dissolved, the stirring body 60 is inserted from the outside into the dissolution tank 20 to stir the melt. That is, since the stirrer 60 is disposed outside the dissolution tank 20 during the melting step in which undissolved raw materials that may attack the stirrer exist, deterioration of the stirrer 60 can be suppressed. Moreover, the deterioration of the quality of the glass by the component which comprises the stirring body 60 being taken in into a melt can also be suppressed.
  • FIG. 3 is a view showing a mode in which the stirring body 60 is inserted into the dissolution tank 20. While not in the stirring step, the open / close window 235 provided above the melt surface FL in the side wall 231 is closed to seal the inside of the dissolution tank 20. On the other hand, after the dissolution step is completed, immediately before the stirring step. Then, as shown in FIG. 3A, the opening / closing window 235 opens to form the opening / closing port 236, and the stirring member 60 can be inserted.
  • the stirrer 60 in the present embodiment has a rod-like base 61 connected to a drive source, and bends at a substantially right angle at a bent portion 63 provided in the middle of the base 61 to reach the tip 65. .
  • the opening / closing port 236 has a width dimension larger than the length from the bent portion 63 to the distal end portion 65 and a vertical width dimension larger than the diameter of the base portion 61 (usually has a horizontally long shape).
  • the stirring body 60 is inserted in a state where the part from the tip part 65 to the tip part 65 is laid down horizontally (FIG. 3B).
  • the base 61 is rotated and the tip 65 is immersed in the melt (FIG. 3C). Thereafter, by operating the drive source, the tip 65 moves in the melt, and the melt is mechanically agitated.
  • the lateral width of the opening / closing port 236 should have such a dimension that the opening / closing window 235 does not contact the base 61 when the tip 65 moves in a desired path in the melt.
  • FIG. 4 is a partially enlarged cross-sectional view of the stirring body 60.
  • the stirrer 60 has a refrigerant flow channel 66 therein, a high expansion ceramic 67 is provided around the refrigerant flow channel 66, and the high expansion ceramic 67 is covered with platinum or a platinum rhodium alloy 68. preferable. Since platinum or the platinum rhodium alloy 68 is excellent in stability, the stirring can be performed while suppressing the mixing of foreign matters into the melt, and the deterioration of the stirring body 60 can be suppressed by the coolant flowing through the coolant channel 66.
  • the amount of platinum or platinum rhodium alloy used can be reduced to reduce the manufacturing cost, and high expansion ceramics are used as the ceramic.
  • high expansion ceramics refers to ceramics whose expansion characteristics under the temperature conditions in the stirring step are similar to those of platinum or platinum rhodium alloy, and are appropriately selected according to the temperature conditions. Al 2 O 3 —CaO based ceramics can be used.
  • coolant flow path 66 is not specifically limited, Liquids, such as water and oil, and gas, such as air, may be sufficient.
  • the feeder 30 can start and stop the outflow by an outflow control means (not shown), communicates the melting tank 20 to the outside world, and guides the molten glass in the melting tank 20 to the mold 50. Specifically, molten glass flows into the communication port 33 facing the melt and is led out from the outlet 35 to the molding die 50 through the main body 31.
  • a feeder 30 is formed of platinum or a platinum alloy so as to suppress foreign matters from being mixed into the molten glass.
  • the feeder 30 is preferably provided at the bottom portion 233 of the melting tank 20 and more preferably provided at substantially the center of the bottom portion 233 in that molten glass with higher homogeneity can be derived.
  • the approximate center of the bottom is a similarity in which, in the projection of the bottom along the vertical axis direction of the dissolution tank 20, the center of gravity of the projection of the bottom coincides with the center of gravity, and the area is 10% of the area of the projection of the bottom. It refers to any point in the area surrounded by the shape.
  • the communication port 33 of the feeder 30 is preferably arranged above the bottom portion 233 in that molten glass with higher homogeneity can be derived.
  • the electrodes 21a to 21d, 21 ′ are not so hindered from energizing heating. It must be located below the installation height of a to 21'd.
  • the mold 50 molds molten glass led out from the feeder 30.
  • the mold 50 has a size that matches the desired size of the glass molded body. For example, when a large volume glass block is desired, the large volume mold 50 is used.
  • the manufacturing method of the glass molded object using the above manufacturing apparatus 10 it is preferable to apply the manufacturing method of the glass molded object using the above manufacturing apparatus 10 to manufacture of the glass molded object whose viscosity of the melt in the highest temperature during a heating process is 1.5 poise or more.
  • the lower limit of the melt viscosity at the highest temperature during the heating step is more preferably 1.7 poise, most preferably 1.8 poise.
  • melt viscosity is excessive, the viscosity of the melt at the highest temperature during the heating process, taking into account that manufacturing costs are likely to increase as a result of the enormous energy required for convection and mechanical stirring.
  • the upper limit of is preferably 3.0 poise, more preferably 2.8 poise, and most preferably 2.7 poise.
  • the OH group content of the glass molded body thus obtained is 570 ppm or less.
  • Such a glass molded body is useful as a low expansion glass product excellent in heat resistance.
  • the upper limit of the OH group content in the glass molded body is more preferably 540 ppm, and most preferably 500 ppm.
  • the lower limit of the OH group content of the glass molded body is preferably 50 ppm, more preferably 150 ppm, most preferably 200 ppm.
  • the OH group content in the glass molded body can be calculated using the following Lambert-Beer equation.
  • C log 10 (Ta / Tb) / ⁇ t (In the formula, C is the content (ppm) of OH molecules, and ⁇ is the molar absorption coefficient of water (8.6 L). / Mol ⁇ mm), t is the thickness of the polished glass (mm), Ta and Tb are the transmissivity (%) at each wavelength, and more specifically, Ta is a maximum value near a wavelength of 2.0 ⁇ m. Tb is a transmittance showing a minimum value in the vicinity of a wavelength of 2.21 ⁇ m. )
  • the glass molded body is preferably made of a SiO 2 —Al 2 O 3 —Li 2 O system.
  • a SiO 2 —Al 2 O 3 —Li 2 O-based glass molded body is a low-expansion glass molded body that is useful for many purposes such as an exposure apparatus for semiconductor manufacturing and an astronomical telescope. It is also known that the viscosity of the melt is extremely high.
  • the raw material can be quickly and sufficiently used by combining the heating from above with the combustion burners 41a and 41b and the current heating with the electrodes 21a to 21d and 21'a to 21'd.
  • the production method of the present invention is also suitable for producing amorphous glass for hard disk substrates, crystallized glass for hard disk substrates, and crystallized glass for optical communication filters, which are made of SiO 2 —Li 2 O.
  • the temperature conditions in each step are preferably set to the following values.
  • the temperature of the internal space of the dissolution tank 20 is set to 1530 to 1550 ° C. by the heating unit 40 so that the melt can be obtained quickly. It is preferable to do.
  • the melt in the dissolution tank 20 should not be less than a certain amount unless the glass composition is changed. That is, the amount of melt is controlled so that a certain amount of melt remains in the melting tank 20 even after the amount of molten glass necessary for manufacturing one glass block has flowed out.
  • the raw materials are supplied and melted in the melt until a certain level is reached (dissolution process).
  • the temperature in this step is preferably 1450 ° C. to 1550 ° C., more preferably 1460 ° C. to 1540 ° C., and most preferably 1480 so that the deterioration and undissolved platinum (cause of foreign matter) can be suppressed. ° C to 1500 ° C.
  • the temperature in this step is preferably 1480 ° C. to 1580 ° C., more preferably 1500 ° C. from the viewpoint of reducing combustion energy by the heating unit 40 and suppressing crystal precipitation on the glass surface in the upper part of the melt. It is ⁇ 1560 ° C., most preferably 1510 ° C. to 1540 ° C.
  • the temperature at the bottom of the melt is preferably 1530 ° C. to 1600 ° C., more preferably 1540 ° C. to 1595 ° C., and most preferably so that homogenization of the melt by convection can be promoted and platinum deterioration can be suppressed. 1550 ° C to 1590 ° C.
  • Example 1 Using the glass molded body manufacturing apparatus 10 described above, 54.5 to 57% SiO 2 component, 6.0% to 8.5% P 2 O 5 component, 22.0 to 20 % by mass based on the oxide. 26.0% Al 2 O 3 component, 3.5-4.2% Li 2 O component, 0.6-1.6% MgO component, 0.4-1.4% ZnO component, 0 0.7-2.0% CaO component, 0.6-1.7% BaO component, 1.6-2.7% TiO 2 component, 1.0-2.2% ZrO 2 component, and A batch raw material containing 0.8 to 1.2% As 2 O 3 component is charged, and oxygen is supplied to the combustion burners 41a and 41b with a height H from the bottom 233 of the dissolution tank 20 to the liquid level of 976 mm.
  • the stirring body 60 was inserted, and clarification and stirring were performed.
  • the melt temperature is a temperature sensor provided with a height of 750 mm from the bottom 233 (the detected value is referred to as an upper temperature), and a temperature within an electrode provided with a height of 230 mm from the bottom 233.
  • the upper temperature was 1516-1530 ° C
  • the lower temperature was 1580-1589 ° C
  • the lower temperature was higher than the upper temperature with a temperature difference of about 60 ° C. .
  • the volume (A) above the melt level FL in the dissolution tank 20 is 2.766 m 3
  • the melt volume (B) is 3.281 m 3
  • A: B 1.19. : 1.
  • the height difference between the center position of the opening of the combustion burner and the liquid level was 612 mm.
  • the raw material supply amount b was 1020 (L), the combustion amount a per unit time was 240000 (kcal / h), and a / b was 235.2.
  • the height h up to the top of the plurality of electrodes was 400 mm. Since the number c of electrodes was 8, b / c was 127.5.
  • the molten glass obtained in this manner was led out to a molding die 50 and slowly cooled after molding to produce a glass molded body having a diameter of 1700 mm and a thickness of 400 mm.
  • the stirrer 60 was rotated until the molten glass was led out to the mold 50, and returned to the outside of the melting tank 20 after the molten glass was led out.
  • the glass molded body was cut to a thickness of about 10 mm, and a polarizing adhesive film was adhered to the surface of the cut piece, and then a surface image was obtained with graphic software. The result is shown in FIG. Further, the OH group content in the glass molded body was 424 to 566 ppm as calculated based on the above-mentioned Lambert-Beer equation.
  • Example 1 A glass molded body is manufactured in the same manner as in Example 1 except that the electrodes 21a to 21d and 21'a to 21'd are not installed, and a manufacturing apparatus having the same configuration as the manufacturing apparatus 10 is used. did. The upper temperature during dissolution, clarification, and stirring was 1602-1604 ° C., and the lower temperature was 1544-1546 ° C. The upper temperature was higher than the lower temperature. Thereby, it is estimated that the convection of the melt is not performed. A surface image of the cut piece is shown in FIG.
  • Example 1 As shown in FIG. 7, it was found that the glass molded body produced in Example 1 was homogeneous and striae were extremely suppressed. In contrast, as shown in FIG. 6, the glass molded body produced in Comparative Example 1 was found to have low homogeneity and striae.
  • the transmittance was measured using a 270-30 type infrared spectrophotometer manufactured by Hitachi, Ltd. using a glass molded body polished to a thickness of 10 mm before crystallization heat treatment as a sample, and the wavelength was around 2.0 ⁇ m.
  • the maximum value of the transmittance is Ta
  • the minimum value of the transmittance around the wavelength of 2.21 ⁇ m is Tb.
  • Reference Example 2-1 uses a manufacturing apparatus with four electrodes (the horizontal cross section of the lower furnace wall 23 is square), and Reference Examples 2-2 to 2-7 have a manufacturing apparatus with eight electrodes (lower part).
  • a glass molded body was manufactured in the same procedure as in Example 1 except that the horizontal cross section of the furnace wall 23 was a regular octagon) and the conditions shown in Table 1 were changed.
  • the stirring time was set shorter than in the other reference examples, and the stirring time was set to 3/5 of the other reference examples.
  • Comparative Example 2 In Comparative Example 2, a glass molded body was produced in the same procedure as in Reference Example 2-1, except that stirring was not performed.
  • Table 1 also shows the OH group content, the degree of striae, and the degree of contamination of the glass molded bodies produced in Reference Example 2 and Comparative Example 2.
  • the standard of striae means ⁇ : not observed at all, ⁇ : almost not observed, ⁇ : observed slightly, x: generated a lot, respectively.
  • the surface image of the glass molded body after crystallization in which the OH group content was 778 ppm and 548 ppm, was obtained.
  • the results are shown in FIG. 8 ((a) corresponds to 778 ppm and (b) corresponds to 548 ppm).
  • FIG. 8 it was confirmed that the glass molded body having an OH group content of 778 ppm was cracked, but the glass molded body having an OH group content of 548 ppm was confirmed to be cracked. could not. Thereby, it was confirmed that generation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Vertical, Hearth, Or Arc Furnaces (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention porte sur un procédé de fabrication d'un corps formé de verre et sur un dispositif de fabrication qui peut supporter la formation d'un bloc de verre de grand volume et améliorer entièrement l'homogénéité du verre. Un dispositif (10) de fabrication d'un corps formé de verre est doté d'un réservoir de fusion (20) dans lequel une masse fondue d'une matière première est reçue et qui comprend plusieurs électrodes (21a, 21'a) immergées dans la masse fondue, un dispositif d'alimentation (30) qui communique avec le réservoir de fusion (20), une unité de chauffage (40) disposée dans la partie supérieure du réservoir de fusion (20), une filière de formage (50) pour former du verre fondu sortant du dispositif d'alimentation (30), et un corps d'agitation (60) pouvant être introduit dans le réservoir de fusion (20) et retiré de celui-ci. Le verre fondu est fabriqué par chauffage de la solution fondue par dessus la solution fondue par l'unité de chauffage (40) tout en chauffant de façon conductrice la solution fondue par connexion électrique des différentes électrodes (21a, 21'a), introduction du corps d'agitation (60) dans le réservoir de fusion (20) de l'extérieur une fois la matière première fondue, et agitation de la solution fondue par le corps d'agitation (60).
PCT/JP2009/061851 2008-06-30 2009-06-29 Procédé de fabrication d'un corps formé de verre et dispositif de fabrication WO2010001857A1 (fr)

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CN115367999A (zh) * 2022-09-21 2022-11-22 成都光明光电股份有限公司 间隙式光学玻璃生产方法及其装置

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CN103570240B (zh) * 2012-07-29 2016-04-06 苏州宏久航空防热材料科技有限公司 一种降低离心棉熔池漏板处玻璃熔体粘度的装置及其方法
WO2017116978A1 (fr) * 2015-12-29 2017-07-06 Kurion, Inc. Système et procédé pour ensemble joint d'électrode
CN107857462A (zh) * 2017-12-18 2018-03-30 山东聚源玄武岩纤维股份有限公司 一种用于生产玄武岩连续纤维的气电窑炉
CN109399942A (zh) * 2018-11-22 2019-03-01 宁波荣山新型材料有限公司 一种泡沫玻璃陶瓷复合建筑保温隔热材料及其制备方法
GB2583093B (en) 2019-04-15 2021-05-12 Glassflake Ltd A system and method for melting materials
EP3760595A1 (fr) * 2019-07-04 2021-01-06 International Partners in Glass Research (IPGR) e.V. Four de fusion de verre
CN113024090A (zh) * 2019-12-24 2021-06-25 江苏康姆罗拉特种陶瓷有限公司 一种石英晶体成型设备
JP2022088071A (ja) * 2020-12-02 2022-06-14 日本電気硝子株式会社 ガラス溶融炉監視方法、及びガラス物品製造方法
CN113562959A (zh) * 2021-06-30 2021-10-29 陕西彩虹工业智能科技有限公司 一种柔性玻璃窑炉烟道结构
KR102649011B1 (ko) * 2022-01-04 2024-03-18 한국수력원자력 주식회사 유리화설비의 원격재기동 시스템 및 그 운용방법

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CN112520978B (zh) * 2020-11-24 2022-11-15 重庆市渝琥玻璃有限公司 循环式冷却搅拌设备
CN115367999A (zh) * 2022-09-21 2022-11-22 成都光明光电股份有限公司 间隙式光学玻璃生产方法及其装置

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