WO2022091657A1 - Procédé de production d'une feuille de verre, feuille de verre, dispositif et équipement de production de feuille de verre - Google Patents

Procédé de production d'une feuille de verre, feuille de verre, dispositif et équipement de production de feuille de verre Download PDF

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Publication number
WO2022091657A1
WO2022091657A1 PCT/JP2021/034876 JP2021034876W WO2022091657A1 WO 2022091657 A1 WO2022091657 A1 WO 2022091657A1 JP 2021034876 W JP2021034876 W JP 2021034876W WO 2022091657 A1 WO2022091657 A1 WO 2022091657A1
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Prior art keywords
glass
glass preform
glass sheet
preform
width
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PCT/JP2021/034876
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English (en)
Japanese (ja)
Inventor
陽 田中
ヤシャイラ ヤリクン
諭 天谷
ヤーポン エン
アイサン ユスフ
キゴウ シン
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国立研究開発法人理化学研究所
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Priority to JP2022558925A priority Critical patent/JPWO2022091657A1/ja
Publication of WO2022091657A1 publication Critical patent/WO2022091657A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00—Re-forming shaped glass
    • C03B23/02—Re-forming glass sheets
    • C03B23/037—Re-forming glass sheets by drawing

Definitions

  • the present invention relates to a method for manufacturing a glass sheet, a glass sheet, a device, and a device for manufacturing a glass sheet.
  • Glass sheets with a thickness of several hundred ⁇ m or less are flexible and are therefore used in various devices such as detectors and optical components.
  • Patent Documents 1 and 2 describe a method for producing an ultrathin glass sheet by heating and stretching a preform (base glass).
  • the preform is heated to the vicinity of the softening point to stretch the softened preform.
  • the base glass is stretched by heating the base glass to a temperature at which the viscosity of the base glass is 107.4 to 108.4 dPa ⁇ s.
  • a glass sheet having a minimum thickness of 10 ⁇ m is obtained.
  • Patent Document 3 describes a fluid control device for a microchip using a thin glass plate having a thickness of 5 to 6 ⁇ m.
  • a thinner glass sheet for various devices such as pressure sensors, microfluidic devices, glass filters, and flexible devices.
  • an object of the present invention is to provide a method for manufacturing a glass sheet capable of manufacturing a thinner glass sheet, a glass sheet obtained by the method, a device using the same, and a glass sheet manufacturing apparatus.
  • the present invention is a method for manufacturing a glass sheet. Including the step of stretching the glass preform to obtain the glass sheet. In the stretching step, the method of pulling the glass preform in the first direction while heating the glass preform to a temperature at which the glass preform has a viscosity in the range of 109 to 10 14 dPa Provided.
  • the second aspect of the present invention is a method for manufacturing a glass sheet. Including the step of stretching the glass preform to obtain the glass sheet.
  • the glass preform is subjected to the following formula (1).
  • Ps represents the strain point of the glass preform.
  • Ts represents the softening point of the glass preform.
  • ⁇ , ⁇ , ⁇ , and ⁇ are 1, 0, 1/5, and 4/5, respectively
  • Provided is a method of pulling the glass preform in a first direction while heating to a temperature T that satisfies.
  • the present invention is a method for manufacturing a glass sheet. Including the step of stretching the glass preform to obtain the glass sheet by pulling the glass preform in the first direction while heating the glass preform.
  • the glass preform has a width of 10 to 1000 mm and has a width of 10 to 1000 mm.
  • a method is provided in which the glass sheet has a thickness of 0.1 or more and less than 10 ⁇ m.
  • a glass sheet having a thickness of 100 nm or more and less than 4 ⁇ m is provided.
  • a glass sheet having a width of more than 2 mm and a width of 4 mm or less and a thickness of 100 nm to 16 ⁇ m is provided.
  • the device provided with the glass sheet of the fourth or fifth aspect is provided.
  • the seventh aspect of the present invention is a glass sheet manufacturing apparatus.
  • the first holder that supports the first part of the glass preform, A second holder that contacts the second portion of the glass preform and provides a force that pulls the glass preform between the first and second portions in the first direction.
  • a heater that heats the glass preform and A controller that controls the temperature of the heater and Equipped with The controller controls the heater so that the heater heats the glass preform to a predetermined temperature.
  • An apparatus is provided in which the glass preform has a viscosity in the range of 10 9 to 10 14 dPa at the predetermined temperature.
  • the manufacturing method and manufacturing apparatus of the present invention make it possible to manufacture an ultra-thin glass sheet. Further, the glass sheet of the present invention is useful for various devices such as pressure sensors.
  • FIG. 1 is a schematic diagram for explaining the manufacturing method according to the first embodiment.
  • FIG. 2 is a schematic view showing an example of a pressure sensor using a glass sheet manufactured by the manufacturing method according to the first embodiment.
  • FIG. 3 is a schematic view showing an example of a pressure sensor using a glass sheet manufactured by the manufacturing method according to the first embodiment, and shows a state in which the glass sheet is bent.
  • FIG. 4 is a schematic perspective view of an assembly manufactured by adhering a first holder and a second holder of the manufacturing apparatus according to the second embodiment to a glass preform.
  • FIG. 5 is a schematic view of the manufacturing apparatus according to the second embodiment.
  • FIG. 6 is a schematic view of the manufacturing apparatus according to the second embodiment.
  • FIG. 7 is a schematic view of the manufacturing apparatus according to the third embodiment.
  • FIG. 8 is a graph showing the relationship between the width and the thickness of the glass sheets produced in Examples 2 to 8.
  • FIG. 9 is a graph showing the relationship between the width of the glass preform used in Examples 9 to 12 and the thickness of the obtained glass sheet.
  • FIG. 10 is a graph showing the relationship between the applied pressure and the amount of bending of the glass sheet of the pressure sensor produced in Example 17.
  • the method for producing a glass sheet according to the first embodiment includes a step of stretching a glass preform to obtain the glass sheet.
  • first direction the glass preform 10 is pulled and stretched in the direction of the broken line arrow in FIG. 1 (hereinafter referred to as “first direction”).
  • first direction the glass sheet 15 thinner than the glass preform 10 is obtained.
  • the glass sheet means a self-supporting glass film.
  • self-supporting means that the structure itself can be maintained (that is, does not collapse) without constant contact with a support member such as a substrate. Therefore, the glass sheet can be handled independently without the support member, and is formed on the surface of the support member by various film forming methods such as a vapor deposition method and a coating method, which are held by the support member. It is clearly distinguished from the glass film).
  • any glass such as borosilicate glass, quartz glass, soda lime glass, non-alkali glass and the like can be used for the glass preform 10.
  • the shape of the glass preform 10 is not particularly limited, but it may be substantially rectangular.
  • the glass preform 10 may have an arbitrary thickness depending on the dimensions of the glass sheet 15 to be manufactured, and may have a thickness in the range of, for example, 10 to 700 ⁇ m.
  • the glass preform 10 having a thickness of 30 ⁇ m or more can be produced by a general method such as polishing and can be easily obtained from the market.
  • the glass preform 10 has a thickness of 500 ⁇ m or less, it is possible to manufacture a sufficiently thin glass sheet 15.
  • the glass preform 10 may have an arbitrary width depending on the dimensions of the glass sheet 15 to be manufactured.
  • the glass preform 10 may have a width in the range of 10 to 2000 mm or 10 to 1000 mm, but is not limited to this.
  • the glass preform 10 has a width within the above range, it is possible to manufacture a sufficiently thin glass sheet 15.
  • the glass preform 10 may have an arbitrary length depending on the dimensions of the glass sheet 15 to be manufactured.
  • the glass preform 10 may have a length in the range of, for example, 1 mm to 10 cm, 2 mm to 8 cm, or 3 mm to 5 cm. , Not limited to this.
  • the glass preform 10 is, for example, 1 to 5000 m, 1 to 3000 m, 1 to 1000 m, 2 to 800 m, 2 to It may have a length of 600m, 2-400m, 2-200m, 2-100m, 3-80m, 3-60m, 3-40m, 3-20m, or 3-10m, but is not limited thereto.
  • the glass preform 10 has a viscosity in the range of 10 9 to 10 14 dPa, 10 9 to 10 13 dPa, 10 9 to 10 12 dPa, or 10 9 to 10 11 dPa.
  • the glass preform 10 is heated to a temperature.
  • the temperature range in which the viscosity of the glass preform 10 is within the above range is determined by the fiber stretching method according to ISO7884-3: 1987 using the same material as the material of the glass preform 10.
  • the viscosity of the glass preform 10 By setting the viscosity of the glass preform 10 to 109 dPa or more, the possibility of the glass preform 10 breaking during stretching can be reduced. By setting the viscosity of the glass preform 10 to 10 14 dPa or less, the glass preform 10 can be stretched within a time reasonable for production (for example, within 20 hours).
  • the glass preform 10 is expressed by the following formula (1).
  • Ps represents the strain point of the glass preform 10.
  • Ts represents the softening point of the glass preform 10.
  • ⁇ , ⁇ , ⁇ , and ⁇ are 1, 0, 1/5, 4/5, or 1, 0, 1/4, 3/4, respectively.
  • ⁇ , ⁇ , ⁇ , and ⁇ are 13/14, 1/14, 1/5, 4/5, or 13/14, 1/14, 1/4, 3/4, respectively.
  • ⁇ , ⁇ , ⁇ , and ⁇ are 7/9, 2/9, 1/5, 4/5, or 7/9, 2/9, 1/4, and 3/4, respectively.
  • ⁇ , ⁇ , ⁇ , and ⁇ are 9/14, 5/14, 1/5, 4/5, or 9/14, 5/14, 1/4, 3/4, respectively.
  • ⁇ , ⁇ , ⁇ , and ⁇ are 1/2, 1/2, 1/5, 4/5, or 1/2, 1/2, 1/4, 3/4, respectively.
  • the heated glass preform 10 can have an appropriate viscosity, the possibility that the glass preform 10 breaks during stretching is reduced, and the glass is manufactured within a reasonable time (for example, within 20 hours).
  • the preform 10 can be stretched.
  • the strain point Ps of the glass preform 10 is obtained according to JIS R3103-2: 2001.
  • the softening point Ts of the glass preform 10 is determined according to JIS R 3103-1: 2001.
  • the heating temperature of the glass preform 10 may be 40 ° C. or higher lower than the softening point of the glass preform 10. Thereby, the possibility that the glass preform 10 is broken during stretching can be reduced.
  • the heating method of the glass preform 10 is not particularly limited.
  • the glass preform 10 may be placed in a heating furnace and heated.
  • the atmosphere during heating is not particularly limited, and may be, for example, an air atmosphere, an inert atmosphere, or a vacuum atmosphere. When heating in a vacuum furnace, the cooling rate of the glass preform 10 can be easily controlled.
  • the first direction for pulling the glass preform 10 may be any direction, but in particular, it may be the direction of gravity. Thereby, when the glass preform 10 is stretched, it is possible to prevent the glass preform 10 from bending due to its own weight.
  • the magnitude of the pulling force of the glass preform 10 may be appropriately set according to the dimensions of the glass preform 10 and the glass sheet 15 to be manufactured, the heating temperature, and the like.
  • the glass preform 10 is stretched by pulling the glass preform 10 having a viscosity within the above range with a force of an appropriate magnitude. As a result, the glass sheet 15 thinner than the glass preform 10 is formed.
  • the stretching time may be appropriately set according to the dimensions of the glass preform 10 to be used and the glass sheet 15 to be manufactured, the heating temperature of the glass preform 10, the magnitude of the pulling force, and the like. It may be hours or more, 2.5 hours or more, 3 hours or more, or 4 hours or more. By slowly stretching the glass preform 10 over such a long time, it is possible to prevent the glass preform 10 having a high viscosity of 109 dPa or more from breaking during stretching. Further, from the viewpoint of production efficiency, the stretching time may be 20 hours or less.
  • the glass sheet 15 obtained by stretching may be cooled to room temperature. During cooling, the temperature may be controlled so that the glass sheet 15 is slowly cooled. By slowly cooling the glass sheet 15, distortion of the glass sheet 15 can be suppressed.
  • the manufactured glass sheet 15 is typically in the shape of a long ribbon.
  • the glass sheet 15 may have a length of 1 mm or more, 2 mm or more, or 10 mm or more.
  • the glass sheet 15 has a thickness and width smaller than that of the glass preform 10 and a length longer than that of the glass preform 10.
  • the ratio of the width to the thickness of the glass sheet 15 (hereinafter, appropriately referred to as “aspect ratio of the glass sheet 15”) is the ratio of the width to the thickness of the glass preform 10 (hereinafter, appropriately referred to as “aspect ratio of the glass preform 10”). It may be 0.6 to 1.1 times, 0.7 to 1.05 times, or 0.9 to 1.05 times.
  • the aspect ratio of the manufactured glass sheet 15 is approximately equal to the aspect ratio of the glass preform 10. As shown in Examples described later, when the width of the glass sheet 15 exceeds 2 mm, the smaller the width of the glass sheet 15, the thinner the glass sheet 15. However, when the width of the glass sheet 15 is 2 mm or less, the smaller the width of the glass sheet 15, the thicker the glass sheet 15 (see FIG. 8). In order to efficiently produce the ultrathin glass sheet 15, the glass sheet 15 may have a width within the range of 1 to 10 mm, 1 to 5 mm, 2 to 4 mm, or more than 2 mm and 4 mm or less.
  • the glass sheet 15 may have a thickness of 100 nm or more and less than 30 ⁇ m, 100 nm or more and 16 ⁇ m or less, 100 nm or more and less than 10 ⁇ m, 100 nm or more and less than 4 ⁇ m, 100 nm or more and 3 ⁇ m or less, 100 nm or more and 2 ⁇ m or less, or 100 nm or more and 1 ⁇ m or less. ..
  • the manufacturing method according to the first embodiment makes it possible to manufacture a glass sheet 15 having a thickness of 100 nm or more and less than 4 ⁇ m, which could not be manufactured by the conventional manufacturing method.
  • the manufacturing method according to the first embodiment also makes it possible to manufacture a glass sheet 15 having a width of more than 2 mm and a width of 4 mm or less and a thickness of 100 nm to 16 ⁇ m.
  • the glass sheet 15 having such a small width and thickness could not be manufactured by the conventional method.
  • the manufacturing method according to the first embodiment enables the manufacturing of an ultra-thin glass sheet 15.
  • the ultra-thin small glass sheet 15 can be used for various devices such as pressure sensors, microfluidic devices as described in Patent Document 3, glass filters, flexible devices, and the like, thereby reducing the size of these devices. , And the sensitivity and performance can be improved. Further, since the glass sheet 15 has higher chemical stability than the resin sheet, it can be applied to a device in which various liquids such as an acidic solution and an organic solvent are used. Further, since the glass sheet 15 has high transparency, it is also advantageous in optical applications.
  • FIG. 2 and 3 show a schematic cross-sectional view of the pressure sensor 5, which is an example of the use of the glass sheet 15.
  • a plate-shaped first member 210 having a through hole 212, a glass sheet 15, and a second member 230 having a through hole 232 are laminated in this order.
  • the glass sheet 15 covers the through holes 212 and 232.
  • the first member 210 and the second member 230 may be formed of a material such as glass or PDMS.
  • FIG. 3 when there is a difference in the pressure applied to both sides of the glass sheet 15, the glass sheet 15 bends. The amount of bending ⁇ of the glass sheet 15 depends on the pressure difference.
  • the pressure difference can be obtained by measuring the amount of deflection ⁇ with a measuring microscope or the like.
  • the glass filter can be manufactured, for example, by forming a plurality of holes having a diameter of several ⁇ m or less on the glass sheet 15 with a laser. Since such a glass filter can allow air to pass through without allowing fluid to permeate, it can be used for applications such as cell culture.
  • Second embodiment (glass sheet manufacturing apparatus)
  • the manufacturing apparatus according to the second embodiment is an example of a batch type manufacturing apparatus used in the manufacturing method according to the first embodiment.
  • the second embodiment will be described with reference to FIGS. 4, 5 and 6.
  • the glass sheet manufacturing apparatus 1 comes into contact with the first holder 30 that supports the first portion 11 of the glass preform 10 and the second portion 12 of the glass preform 10, and the first portion 11 A second holder 50 that gives a force to pull the glass preform 10 between the glass preform 10 and the second portion 12 in the first direction, a heater 80 that heats the glass preform 10, and a controller that controls the temperature of the heater 80 (not shown). ) And.
  • the first portion 11 of the glass preform 10 may be the first end of the glass preform, and the second portion 12 may be the second end opposite to the first end.
  • the first holder 30 and the second holder 50 may be made of any heat-resistant material such as carbon, stainless steel, and heat-resistant glass.
  • the first holder 30 and the second holder 50 may be plate-shaped, but are not limited thereto.
  • the first holder 30 may be provided with a structure (for example, a through hole 32) for fixing to the fixing base 90 described later.
  • the glass preform 10 is fixed to the first holder 30 and the second holder 50 by any method.
  • the first holder 30 supports the first portion 11 of the glass preform 10, and the second holder 50 comes into contact with the second portion 12 of the glass preform 10.
  • the first portion 11 of the glass preform 10 may be fixed to the first holder 30 and the second portion 12 may be fixed to the second holder 50 using a heat-resistant adhesive.
  • the weight 70 is connected to the second holder 50.
  • the weight of the second holder 50 and the weight 70 provides a force that pulls the glass preform 10 between the first portion 11 and the second portion 12 in the first direction.
  • the weight 70 may be made of any heat-resistant material such as carbon or stainless steel.
  • the method of connecting the weight 70 to the second holder 50 is not particularly limited, but the weight 70 may be fixed to the second holder 50 by using, for example, a heat-resistant adhesive.
  • the weight 70 is not essential, and a force for pulling the glass preform 10 in the first direction may be applied only by the weight of the second holder 50.
  • the first direction is the direction of gravity.
  • the heater 80 for heating the glass preform 10 may be provided in the heating furnace.
  • a fixing table 90 may be further arranged in the heating furnace.
  • the fixing base 90 may be formed of any heat-resistant material such as carbon, stainless steel, and heat-resistant glass.
  • the first holder 30 is fixed to the upper part of the fixing base 90.
  • the fixed base 90 is manufactured so that the second holder 50 does not come into contact with the fixed base 90 or the bottom of the heating furnace when the glass preform 10 is stretched to prepare the glass sheet 15 (see FIG. 6). Has a sufficient height H depending on the length of the glass.
  • the temperature of the heater 80 is controlled by a controller (not shown).
  • the heater 80 is set to a temperature at which the glass preform 10 has a viscosity in the range of 10 9 to 10 14 dPa, 10 9 to 10 13 dPa, 10 9 to 10 12 dPa, or 10 9 to 10 11 dPa. 10 is heated.
  • the heater 80 heats the glass preform 10 to a temperature T that satisfies the above formula (1).
  • the heater 80 may heat the glass preform 10 to a temperature 40 ° C. or higher lower than the softening point of the glass preform 10. As shown in FIG. 6, the heated glass preform 10 is pulled and stretched in the direction of gravity by the weight of the second holder 50 and the weight 70 to form the glass sheet 15.
  • the output of the heater 80 may be controlled by a controller so that the glass sheet 15 is gradually cooled.
  • FIGS. 5 and 6 show an apparatus for manufacturing one glass sheet 15 in one batch, a plurality of glass preforms 10 are arranged in a heating furnace, and a plurality of glasses in one batch. Sheet 15 may be manufactured.
  • the manufacturing apparatus according to the third embodiment is an example of a continuous type (roll-to-roll type) manufacturing apparatus used in the manufacturing method according to the first embodiment.
  • the third embodiment will be described with reference to FIG. 7.
  • the glass sheet manufacturing apparatus 100 includes a feeding roll 170 for feeding out the glass preform 110, a winding roll 190 for winding the glass preform 10, and a glass preform 110.
  • a pair of upstream nip rolls 132, 134 as first holders supporting the first portion 111, contacting the second portion 112 of the glass preform 110, and the glass preform between the first portion 111 and the second portion 112.
  • a pair of downstream nip rolls 152 and 154 as a second holder that applies a force that pulls the 110 in the first direction, a heater 180 that heats the glass preform 110, and a controller (not shown) that controls the temperature of the heater 180.
  • a pair of upstream nip rolls 132 and 134 are arranged downstream of the feeding roll 170, and a pair of downstream nip rolls 152 and 154 are arranged downstream of the pair of upstream nip rolls 132 and 134.
  • the take-up roll 190 is arranged downstream of the downstream nip rolls 152 and 154. That is, the glass preform 110 is sequentially bridged over the feeding roll 170, the pair of upstream nip rolls 132 and 134, the pair of downstream nip rolls 152 and 154, and the take-up roll 190.
  • the feeding roll 170 has a substantially cylindrical shape, and the glass preform 110 is wound around the outer peripheral surface.
  • the width and diameter of the feeding roll 170 may be appropriately selected depending on the width and flexibility of the glass preform 110.
  • the feeding roll 170 is not essential.
  • the glass preform 110 that is not wound around the roll may be conveyed to the upstream nip rolls 132 and 134 as it is.
  • the pair of upstream nip rolls 132, 134 and the pair of downstream nip rolls 152, 154 have a substantially cylindrical shape.
  • the pair of upstream nip rolls 132, 134 and the pair of downstream nip rolls 152, 154 may be made of any heat resistant material such as carbon, stainless steel, and heat resistant glass.
  • the pair of upstream nip rolls 132 and 134 are in contact with the first portion 111 of the glass preform 110 and are arranged so as to face each other with the glass preform 110 interposed therebetween. Thereby, the pair of upstream nip rolls 132, 134 support the first portion 111 of the glass preform 110.
  • the pair of downstream nip rolls 152 and 154 are arranged in contact with the second portion 112 of the glass preform 110 and facing each other with the glass preform 110 interposed therebetween.
  • the pair of downstream nip rolls 152 and 154 rotate at a higher rotational speed than the pair of upstream nip rolls 132 and 134.
  • the pair of downstream nip rolls 152 and 154 exert a force to pull the glass preform 110 between the first portion 111 and the second portion 112 in the first direction.
  • the downstream nip rolls 152 and 154 may be arranged below the pair of upstream nip rolls 132 and 134 in the direction of gravity, in which case the glass preform 110 is pulled in the direction of gravity.
  • the heater 180 heats the glass preform 110 between the first portion 111 and the second portion 112.
  • the heater 180 may be provided in the heating furnace 160.
  • a pair of upstream nip rolls 132, 134 and a pair of downstream nip rolls 152, 154 may also be arranged in the heating furnace 160.
  • the temperature of the heater 180 is controlled by a controller (not shown).
  • the heater 180 is heated to a temperature at which the glass preform 110 has a viscosity in the range of 10 9 to 10 14 dPa, 10 9 to 10 13 dPa, 10 9 to 10 12 dPa, or 10 9 to 10 11 dPa.
  • Heat 110 Alternatively, the heater 180 heats the glass preform 110 to a temperature T that satisfies the above formula (1).
  • the heater 180 may heat the glass preform 110 to a temperature 40 ° C. or higher lower than the softening point of the glass preform 110.
  • the heated glass preform 110 is pulled and stretched in the first direction to form the glass sheet 115.
  • the output of the heater 180 may be controlled by a controller so that the glass sheet 115 is gradually cooled.
  • the formed glass sheet 115 is taken up by a take-up roll 190.
  • the take-up roll 190 has a substantially cylindrical shape, and the glass sheet 115 is wound around the outer peripheral surface.
  • the width and diameter of the take-up roll 190 may be appropriately selected depending on the width and flexibility of the glass sheet 115.
  • the take-up roll 190 is not essential. For example, the product may be obtained by cutting the formed glass sheet 115 to a desired length without winding it.
  • the glass sheet manufacturing apparatus of the present disclosure is not limited to an apparatus in which a first holder, a second holder, a heater, and a controller are integrated, but at least one of the first holder, the second holder, the heater, and the controller.
  • a device system in which one element is combined with the remaining elements as independent elements eg, a device system in which a first holder and a second holder are combined as independent elements in a heating furnace equipped with a heater and a controller). Also includes.
  • Example 1 The following items were prepared as the glass preform, the first holder, and the second holder.
  • -Glass preform borosilicate glass plate with a length of 5 mm, a width of 30 mm, and a thickness of 30 ⁇ m (manufactured by Matsunami Glass Industry Co., Ltd., code number 0100, glass softening point 736 ° C, glass transition point 557 ° C, strain point 529 ° C).
  • 1st holder Heat-resistant borosilicate glass plate (manufactured by Matsunami Glass Industry Co., Ltd., code number Tempax) having two through holes (diameter 6 mm) arranged in the width direction and having a length of 35 mm, a width of 30 mm, and a thickness of 700 ⁇ m.
  • -Second holder heat-resistant borosilicate glass plate with a length of 20 mm, a width of 30 mm, and a thickness of 700 ⁇ m (manufactured by Matsunami Glass Industry Co., Ltd., code number Tempax)
  • a weight (made of stainless steel) was adhered to the second holder using a heat-resistant adhesive, and the total mass of the second holder and the weight was 1 g.
  • the first end and the second end of the glass preform in the length direction were adhered to the first holder and the second holder, respectively, to prepare an assembly as shown in FIG.
  • the first holder was fixed to a carbon fixing base (height 190 mm) arranged in a vacuum gas replacement furnace (KDF-900GL manufactured by Denken Hydental Co., Ltd.).
  • the glass preform was heated to the temperature shown in Table 1 for 2.5 hours. After that, the inside of the furnace was naturally cooled. A similar experiment was performed 5 times. Successful when the glass preform is stretched in the direction of gravity to obtain a glass sheet longer than the glass preform, and failure when the glass preform is not stretched or the glass preform is broken. , The stretching success rate was calculated. The stretching success rate is shown in Table 1.
  • Comparative Example 1 The glass preform was stretched in the same manner as in Example 1 except that the heating temperature of the glass preform was as shown in Table 1, and the stretching success rate was obtained. The results are shown in Table 1.
  • Reference examples 1 to 3 An attempt was made to stretch the glass preform in the same manner as in Example 1 except that the heating temperature of the glass preform was as shown in Table 1. In any of the reference examples, the length of the glass preform did not increase, and the stretching success rate was as shown in Table 1. In Reference Examples 1 to 3 in which the heating temperature was 670 ° C. or lower, the viscosity of the glass preform was higher than that in Example 1. Therefore, in order to stretch the glass preform, the total mass of the second holder and the weight was used. It is probable that it was necessary to make it larger than 1 g.
  • Example 1 where the heating temperature was 690 ° C., which was 40 ° C. or more lower than the softening point of the glass preform, all five experiments were successful. In the comparative example in which the heating temperature was 700 ° C., four out of five experiments were successful, but the glass preform broke once.
  • the glass preform has a viscosity of about 109.3 dPa at 690 ° C and a viscosity of 108.9 dPa at 700 ° C. Therefore, it was shown that the breakability of the glass preform can be reduced by setting the heating temperature of the glass preform to a temperature at which the glass preform has a viscosity of 109 dPa or more. At the heating temperatures of Examples 1 and Reference Examples 1 to 3, the glass preform has a viscosity in the range of 109 to 10 12 dPa .
  • Examples 2-8 The length of the glass preform was set to the length shown in Table 1, the total mass of the second holder and the weight was set to the mass shown in Table 1, and the inside of the furnace was slowly cooled after heating the glass preform.
  • the glass preform was stretched in the same manner as in Example 1 except for the above. As a result, a glass sheet was obtained. Specifically, the slow cooling was performed by cooling to 520 ° C. in 2.5 hours and then naturally cooling.
  • the length, width and thickness of the obtained glass sheet were measured.
  • the length and width of the glass sheet were measured using a ruler, and the thickness of the glass sheet was measured from the cross-sectional SEM image. The measurement results are shown in Table 1.
  • FIG. 8 shows the relationship between the width and the thickness of the obtained glass sheet based on the measurement results. From FIG. 8, it is possible to efficiently manufacture an ultrathin glass sheet by setting the width of the glass sheet within the range of 1 to 10 mm, 1 to 5 mm, 2 to 4 mm, or more than 2 mm and 4 mm or less. Shown. Further, as shown in FIG. 8, when the width of the glass sheet exceeds 2 mm, the smaller the width of the glass sheet, the thinner the glass sheet. On the other hand, when the width of the glass sheet was 2 mm or less, the smaller the width of the glass sheet, the thicker the glass sheet. The inventors consider this reason as follows.
  • the width and thickness values become smaller while the width to thickness ratio (aspect ratio) is maintained due to the elasticity of the glass.
  • the width becomes a predetermined value (here, about 2 mm) or less, the action of the surface tension to reduce the surface area of the glass exceeds the action of the elastic force to maintain the ratio of the width to the thickness. As a result, the thickness of the manufactured glass sheet increases.
  • the width of the glass sheet to be manufactured is within a predetermined range (here, within a range of 1 to 10 mm, 1 to 5 mm, 2 to 4 mm, or more than 2 mm and 4 mm or less)
  • the aspect ratio of the glass preform It was suggested that the higher the ratio, the thinner the glass sheet. That is, among the glass preforms having the same thickness but different widths, the larger the width of the glass preforms, the thinner the glass sheet can be manufactured. In other words, it was suggested that the width of the glass preform and the thickness of the glass sheet are inversely proportional. This was confirmed through Examples 9 to 12 below.
  • the preform was stretched.
  • the widths of the first holder and the second holder were the same as the width of the glass preform.
  • the length, width and thickness of the obtained glass sheet were measured. The measurement results are shown in Table 1.
  • FIG. 9 shows the relationship between the width of the glass preform used in Examples 9 to 12 and the thickness of the obtained glass sheet.
  • the width of the glass preform and the thickness of the glass sheet were approximately inversely proportional.
  • the broken line in FIG. 9 shows an inverse proportional curve extrapolated from the results of Examples 9 to 12.
  • a thinner glass sheet can be made by using a glass preform having a larger width.
  • a glass sheet having a thickness of about 100 nm can be formed by stretching a glass preform having a width of about 800 mm.
  • Example 13 A glass preform was stretched in the same manner as in Example 9 to obtain a glass sheet.
  • the thickness and average surface roughness of the glass sheet were measured at the center of the obtained glass sheet and at a position 3 mm from both ends in the length direction (hereinafter referred to as "near both ends").
  • the thickness of the glass sheet was measured from the cross-sectional SEM image, and the average surface roughness was measured using an atomic force microscope (AFM).
  • AFM atomic force microscope
  • the thickness at the center of the glass sheet was 3.0 ⁇ m, and the thickness near both ends was 3.63 ⁇ m and 3.75 ⁇ m.
  • the average surface roughness in the center of the glass sheet was 1.52 nm, and the average surface roughness in the vicinity of both ends was 1.64 nm and 1.44 nm. From these results, it was shown that the obtained glass sheet had a very small thickness from the center to the vicinity of both ends and had a sufficiently smooth surface.
  • Examples 14 to 15 The following items were prepared as the first holder and the second holder as the glass preform, the total mass of the second holder and the weight was set to the mass shown in Table 1, and the heating temperature of the glass preform and The glass preform was stretched in the same manner as in Example 2 except that the heating time was as shown in Table 1.
  • -Glass preform Non-alkali glass plate with a length of 3 mm, a width of 30 mm, and a thickness of 50 ⁇ m (manufactured by Nippon Electric Glass Co., Ltd., glass softening point 940 ° C, glass transition point 711 ° C, strain point 670 ° C)
  • First holder Quartz glass plate with a length of 20 mm, a width of 30 mm, and a thickness of 0.7 mm (manufactured by Matsunami Glass Industry Co., Ltd.)
  • -Second holder Quartz glass plate with a length of 20 mm, a width of 30 mm, and a thickness of 0.7 mm (manufactured by Matsunami Glass Industry Co., Ltd.)
  • the length, width and thickness of the obtained glass sheet were measured.
  • the measurement results are shown in Table 1. It was confirmed that the glass preform could be stretched at a heating temperature of 865 ° C. and could form a glass sheet having a thickness of 25.5 ⁇ m or less, particularly a very small thickness of 5.1 ⁇ m or less. .. At 865 ° C., the glass preform has a viscosity of about 109.3 dPa.
  • Example 16 The following items were prepared as the glass preform, the first holder, and the second holder, the total mass of the second holder and the weight was set to the mass shown in Table 1, and the heating temperature and heating of the glass preform.
  • the glass preform was stretched in the same manner as in Example 2 except that the time was as shown in Table 1.
  • -Glass preform Quartz glass plate with a length of 2 mm, a width of 30 mm, and a thickness of 50 ⁇ m (manufactured by Shin-Etsu Chemical, glass softening point 1600 ° C, glass transition point 1100 ° C, strain point 1000 ° C)
  • 1st holder Quartz glass plate with a length of 35 mm, a width of 30 mm, and a thickness of 1 mm (manufactured by Shin-Etsu Chemical Co., Ltd.) having two through holes (diameter 6 mm) arranged in the width direction.
  • -Second holder Quartz glass plate with a length of 20 mm, a width of 30 mm, and a thickness of 1 mm (manufactured by Shin-Etsu Chemical Co., Ltd.)
  • the length, width and thickness of the obtained glass sheet were measured. The measurement results are shown in Table 1. It was confirmed that the glass preform was stretched at a heating temperature of 1100 ° C. At 1100 ° C., the glass preform has a viscosity of about 10 13 dPa.
  • Example 17 An orifice with a diameter of 800 ⁇ m was formed on a glass plate having a thickness of 0.7 mm.
  • the glass sheet of Example 9 was fused so as to cover this orifice. Further, a PDMS plate provided with a through hole was adhered to the glass plate.
  • a pressure sensor as shown in FIG. 2 was manufactured. A pressure was applied to the pressure sensor, and the bending amount ⁇ (see FIG. 3) of the glass sheet was measured with a measuring microscope (MF-B1010C manufactured by Mitutoyo Co., Ltd.). The results are shown in FIG.
  • the solid line in FIG. 10 represents the calculated value of the bending amount ⁇ of the glass sheet having a thickness of 3 ⁇ m.
  • the amount of deflection ⁇ with respect to the applied pressure of the prepared pressure sensor was smaller than the calculated value, but the pressure sensor showed good sensitivity to the applied pressure.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)

Abstract

L'invention concerne un procédé de production d'une feuille de verre apte à produire une feuille de verre plus mince, une feuille de verre ainsi obtenue, un dispositif l'utilisant, et un équipement permettant de produire une feuille de verre.　Le procédé de production d'une feuille de verre (15) comprend une étape d'étirage d'une préforme de verre (10) pour obtenir la feuille de verre (15). À l'étape d'étirage, la préforme de verre (10) est étirée dans une première direction tout en chauffant la préforme de verre (10) à une température à laquelle la préforme de verre (10) a une viscosité comprise entre 109 et 1014 dPa.
PCT/JP2021/034876 2020-10-30 2021-09-22 Procédé de production d'une feuille de verre, feuille de verre, dispositif et équipement de production de feuille de verre WO2022091657A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006313343A (ja) * 2005-05-04 2006-11-16 Arisawa Mfg Co Ltd 偏光ガラス及びその製造方法
WO2011016352A1 (fr) * 2009-08-07 2011-02-10 旭硝子株式会社 Procédé de fabrication d'un substrat en verre ultramince
JP2011046593A (ja) * 2009-07-30 2011-03-10 Nippon Electric Glass Co Ltd ガラスリボン及びその製造方法
JP2012087006A (ja) * 2010-10-20 2012-05-10 Nippon Electric Glass Co Ltd ガラスフィルムの製造方法及びガラスフィルム
WO2015198934A1 (fr) * 2014-06-26 2015-12-30 日本電気硝子株式会社 Plaque de verre polarisant et son procédé de fabrication, ensemble de plaque de verre polarisant pour isolateur optique et procédé de fabrication d'un élément optique pour isolateur optique

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006313343A (ja) * 2005-05-04 2006-11-16 Arisawa Mfg Co Ltd 偏光ガラス及びその製造方法
JP2011046593A (ja) * 2009-07-30 2011-03-10 Nippon Electric Glass Co Ltd ガラスリボン及びその製造方法
WO2011016352A1 (fr) * 2009-08-07 2011-02-10 旭硝子株式会社 Procédé de fabrication d'un substrat en verre ultramince
JP2012087006A (ja) * 2010-10-20 2012-05-10 Nippon Electric Glass Co Ltd ガラスフィルムの製造方法及びガラスフィルム
WO2015198934A1 (fr) * 2014-06-26 2015-12-30 日本電気硝子株式会社 Plaque de verre polarisant et son procédé de fabrication, ensemble de plaque de verre polarisant pour isolateur optique et procédé de fabrication d'un élément optique pour isolateur optique

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