JP6578906B2 - Glass material manufacturing method and glass material manufacturing apparatus - Google Patents

Description

  The present invention relates to a glass material manufacturing method and manufacturing apparatus by a containerless floating method.

  In recent years, research on a containerless floating method has been made as a method for producing a glass material. For example, in Patent Document 1, a barium titanium ferroelectric sample suspended in a gas floating furnace is irradiated with a laser beam, heated and melted, and then cooled, whereby the barium titanium ferroelectric sample is cooled to glass. Is described. Thus, in the containerless floating method, since the progress of crystallization due to contact with the wall surface of the container can be suppressed, even a material that could not be vitrified by a conventional manufacturing method using a container. It may be vitrified. Therefore, the containerless floating method is a method that should be noted as a method capable of producing a glass material having a novel composition.

  In Patent Document 2, a larger glass material is obtained by using a containerless floating method using a molding surface having a plurality of gas ejection holes. It is preferable to obtain a large glass material because the variety of application development is increased.

JP 2006-248801 A JP 2014-141389 A

  However, there is a demand for a method capable of producing a larger glass material than the method described in Patent Document 2.

  The objective of this invention is providing the manufacturing method and manufacturing apparatus of the glass material by the containerless floating method which can manufacture a bigger glass material.

  The production method of the present invention is a method of producing a glass material by cooling after heating and melting in a state where the glass raw material lump is suspended in a substantially vertical direction, and in the state where the glass raw material lump is floated and melted Molding in which a plurality of first gas ejection holes positioned in the vicinity of the outer peripheral edge in the substantially horizontal direction of the melt of the raw material lump and a plurality of second gas ejection holes positioned inward from the vicinity of the outer peripheral edge are formed. The step of preparing the member, the step of arranging the glass raw material lump on the molded member, and the state in which the glass raw material lump is suspended by ejecting gas from the first gas ejection hole and the second gas ejection hole In which the gas ejected from the first gas ejection hole is ejected at a flow rate faster than the gas ejected from the second gas ejection hole.

  In this invention, it is preferable that the 1st glass ejection hole is formed in the position 0.8 times-1.5 times the diameter of the substantially horizontal direction of the melt of a glass raw material lump.

  In the present invention, it is preferable that the first glass ejection holes are arranged circumferentially.

  In the present invention, the gas ejected from the first gas ejection hole is ejected from the second gas ejection hole by making the diameter of the first gas ejection hole smaller than that of the second gas ejection hole. The gas is preferably ejected at a flow rate faster than that of the gas.

  The production apparatus of the present invention is an apparatus for producing a glass material by cooling after heating and melting in a state where the glass raw material lump is suspended in a substantially vertical direction by a gas, in a state where the glass raw material lump is floated and melted A plurality of first gas ejection holes located in the vicinity of the outer peripheral edge in the substantially horizontal direction of the melt of the glass raw material lump and a plurality of second gas ejection holes located inward from the vicinity of the outer peripheral edge. A molded member, a gas supply means for supplying gas to the first gas ejection hole and the second gas ejection hole, and a heating means for heating the glass raw material lump, wherein the hole diameter of the first gas ejection hole is: It is characterized by being smaller than the diameter of the second gas ejection hole.

  According to the present invention, a large glass material can be produced by a containerless floating method.

It is typical sectional drawing for demonstrating the manufacturing method (manufacturing apparatus) of one Embodiment of this invention. It is a top view which shows the 1st gas ejection hole and 2nd gas ejection hole in one Embodiment of this invention. It is typical sectional drawing which shows the positional relationship of the glass melt and 1st gas ejection hole in one Embodiment of this invention.

  Hereinafter, preferred embodiments will be described. However, the following embodiments are merely examples, and the present invention is not limited to the following embodiments. Moreover, in each drawing, the member which has the substantially the same function may be referred with the same code | symbol.

  FIG. 1 is a schematic cross-sectional view for explaining a manufacturing method (manufacturing apparatus) according to an embodiment of the present invention. As shown in FIG. 1, the glass raw material block 1 is arranged in a state of floating above the gas ejection surface 10 b of the gas ejection part 10 a of the molding member 10. The gas ejection part 10a is formed with a first gas ejection hole 11 and a second gas ejection hole 12 for ejecting the gas 22 from the gas ejection surface 10b. When the gas 22 is ejected from the first gas ejection hole 11 and the second gas ejection hole 12, the glass raw material lump 1 is suspended in a substantially vertical direction (z direction). By supplying the gas 22 from the gas supply means 21 such as a gas cylinder to the first gas ejection hole 11 and the second gas ejection hole 12, the first gas ejection hole 11 and the second gas ejection hole 12 Gas 22 is ejected.

  The type of the gas 22 is not particularly limited, and may be, for example, air or oxygen, an inert gas such as nitrogen gas, argon gas, or helium gas, or carbon monoxide gas. It may be a reducing gas containing carbon dioxide gas or hydrogen.

  The molded member 10 can be made of, for example, silicon carbide, super steel, stainless steel, duralumin, carbon, or the like. In addition, the gas ejection part 10a may be comprised from these materials, and parts other than the gas ejection part 10a may be comprised from other materials.

  As described above, in a state where the glass raw material lump 1 is floated, the glass raw material lump 1 is heated and melted by being irradiated with laser light from the laser irradiation device 20 which is a heating means, and then cooled. Thus, a glass material is obtained. In the step of heating and melting the glass raw material lump 1 and the step of cooling until the temperature of the glass material becomes at least the softening point or less, at least the gas 22 is continuously ejected, and the glass raw material lump 1 or the glass material is the gas ejection surface. It is preferable not to contact 10b. In addition, the heating method of the glass raw material lump 1 is not specifically limited to the method of irradiating a laser beam. For example, the glass raw material lump 1 may be radiantly heated.

  FIG. 2 is a plan view showing a first gas ejection hole and a second gas ejection hole in an embodiment of the present invention. FIG. 3 is a schematic cross-sectional view showing the positional relationship between the glass melt and the first gas ejection holes in one embodiment of the present invention. In FIG. 3, the arrows shown as the first gas ejection holes 11 and the second gas ejection holes 12 indicate the relative positional relationship between the gas ejection holes, and the lengths of the arrows are The relative flow velocity of the gas ejected from the gas ejection hole is shown.

  As shown in FIGS. 2 and 3, a plurality of first gas ejection holes 11 and a plurality of second gas ejection holes 12 are formed. The first gas ejection holes 11 are located in the vicinity of the outer peripheral edge 2a of the glass melt 2 in a substantially horizontal direction (x direction and y direction). Specifically, the first gas ejection holes 11 are arranged circumferentially along the outer peripheral edge 2 a of the glass melt 2 in a substantially horizontal direction (x direction and y direction). The second gas ejection hole 12 is located inside the vicinity of the outer peripheral edge 2a of the glass melt 2 in a substantially horizontal direction (x direction and y direction). The second gas ejection hole 12 is formed on the inner side than the position of the first gas ejection hole 11. The glass melt 2 is in a state where the glass raw material block 1 shown in FIG. 1 is heated and melted.

  As shown in FIG. 2, in the present embodiment, the diameter of the first gas ejection hole 11 is formed to be smaller than the diameter of the second gas ejection hole 12. Thereby, as shown in FIG. 3, the flow velocity of the gas ejected from the first gas ejection hole 11 becomes faster than the flow velocity of the gas ejected from the second gas ejection hole 12. By making the flow velocity of the gas ejected from the first gas ejection hole 11 faster than the flow velocity of the gas ejected from the second gas ejection hole 12, the flow velocity is increased in the vicinity of the outer peripheral edge 2a of the glass melt 2. Can form walls with fast gas. By forming such a wall, the glass melt 2 can be kept inside the gas wall, and the glass melt 2 in a floating state is displaced to contact the gas ejection surface 10b of the molded member 10 and the like. Can be prevented.

  If the glass melt 2 is enlarged in order to produce a large glass material, the glass melt 2 is displaced and easily contacts the molded member 10 and the like. For this reason, the conventional containerless floating method has a problem that a large glass material cannot be produced. According to the present invention, even if the glass melt 2 becomes large, the glass melt 2 can be held inside the gas wall and the displacement can be suppressed, so that a large glass material can be manufactured.

  In the present embodiment, the diameter of the first gas ejection hole 11 is formed to be smaller than the diameter of the second gas ejection hole 12. The diameter of the first gas ejection hole 11 is preferably in the range of 0.05 to 0.95 times the diameter of the second gas ejection hole 12, and in the range of 0.1 to 0.8 times. More preferably, it is in a range of 0.2 to 0.7 times. By setting it as such a range, the position shift of the glass melt 2 can be suppressed more effectively.

  The diameter of the second gas ejection hole 12 is preferably 3 mm or less, more preferably 2 mm or less, further preferably 1 mm or less, particularly preferably 0.8 mm or less, 0.5 mm Most preferably: Moreover, in this embodiment, the hole diameter of the 1st gas ejection hole 11 is set smaller than the 2nd gas ejection hole 12, and it is preferable that it is 2.85 mm or less, and it is more preferable that it is 2 mm or less. It is further preferably 1 mm or less, particularly preferably 0.8 mm or less, and most preferably 0.4 mm or less. However, if the hole diameters of the first gas ejection hole 11 and the second gas ejection hole 12 are too small, it may be difficult to eject the gas. Accordingly, the diameters of the first gas ejection holes 11 and the second gas ejection holes 12 are preferably 0.01 mm or more, and more preferably 0.05 mm or more.

  As shown in FIG. 2, the plurality of second gas ejection holes 12 are provided so that their centers are located at the vertices of the equilateral triangular lattice. The distance between the centers of the adjacent second gas ejection holes 12 is preferably 0.02 mm to 4 mm, more preferably 0.1 mm to 2 mm, and further preferably 0.2 mm to 1.6 mm. The thickness is preferably 0.2 mm to 0.8 mm. In addition, as shown in FIG. 2, the plurality of first gas ejection holes 11 are arranged circumferentially along the outer peripheral edge 2 a of the glass melt 2. The distance between the centers of the adjacent first gas ejection holes 11 is preferably 0.02 mm to 15 mm, more preferably 0.1 mm to 7 mm, and further preferably 0.2 mm to 5 mm. It is particularly preferably 0.3 mm to 3 mm, and most preferably 0.5 mm to 1.5 mm. A plurality of first gas ejection holes 11 may be provided in the vicinity of the outer peripheral edge 2a of the glass melt 2 in a plurality of concentric circles having different diameters.

  As shown in FIG. 3, the first gas ejection hole 11 is formed in the vicinity of the outer peripheral edge 2 a of the glass melt 2. If the diameter of the glass melt 2 in the substantially horizontal direction (x direction and y direction) is D and the diameter in the substantially horizontal direction of the circumference formed by arranging the first gas ejection holes 11 is d, the diameter d Is preferably 0.8 times to 1.5 times the diameter D, more preferably 0.9 times to 1.4 times, and even more preferably 1.0 times to 1.35 times. By setting it as such a range, the position shift of the glass melt 2 can be suppressed more effectively.

  The flow rate of the gas ejected from the first gas ejection hole 11 is preferably 1.1 to 400 times, more preferably 1.5 times the flow rate of the gas ejected from the second gas ejection hole 12. Double to 100 times, more preferably 2 to 25 times. By setting it as such a range, the position shift of the glass melt 2 can be suppressed more effectively.

  In the present embodiment, by making the diameter of the first gas ejection hole 11 smaller than the diameter of the second gas ejection hole 12, the flow velocity of the gas ejected from the first gas ejection hole 11 is changed to the second. The flow velocity of the gas ejected from the gas ejection hole 12 is faster. The present invention is not limited to this, and the flow rate of the gas ejected from the first gas ejection hole 11 is made higher than that of the gas ejected from the second gas ejection hole 12 by other methods. May be. For example, the flow rate of the gas supplied to the first gas ejection hole 11 is separated from the flow path of the gas supplied to the first gas ejection hole 11 and the flow path of the gas supplied to the second gas ejection hole 12. By making the flow velocity of the gas supplied to the second gas ejection hole 12 faster, the flow velocity of the gas ejected from the first gas ejection hole 11 is made higher than the flow velocity of the gas ejected from the second gas ejection hole 12. May be faster.

  Further, another gas ejection hole may be provided outside the vicinity of the outer peripheral edge 2 a of the glass melt 2. The hole diameter of such a gas ejection hole may be the same as that of the first gas ejection hole 11, may be the same as that of the second gas ejection hole 12, or these gas ejections. The hole diameter may be different from the hole.

  According to the present invention, a large glass material can be produced by a containerless floating method. Therefore, a large glass material can be produced for glass having a composition that does not include a network-forming oxide and does not vitrify by a melting method using a container. Examples of such glasses include terbium-boric acid composite oxide glass materials, barium titanate glass materials, lanthanum-niobium composite oxide glass materials, lanthanum-niobium-aluminum composite oxide glass materials, and lanthanum. -Niobium-tantalum composite oxide glass material, lanthanum-tungsten composite oxide glass material, lanthanum-titanium composite oxide glass material, lanthanum-titanium-zirconia composite oxide glass material, and the like.

  Hereinafter, the present invention will be described in more detail on the basis of specific examples. However, the present invention is not limited to the following examples, and may be appropriately modified and implemented without departing from the scope of the present invention. Is possible.

Example 1
First, after weighing and mixing the raw material powder, the mixed powder was sintered by calcining at a temperature around 1000 ° C. The glass raw material lump 1 was produced by cutting the sintered body into a desired volume.

  Next, using a glass material manufacturing apparatus according to FIGS. 1 and 2, irradiation with a carbon dioxide laser with an output of 100 W is performed with the glass raw material lump levitated above the gas ejection surface 10b under the following conditions. The glass raw material lump 1 was heated and melted. Thereafter, the laser irradiation was stopped and cooled. As a result, a glass material having a diameter of 8.32 mm was obtained.

Glass composition (molar ratio): 0.6 · Tb ₂ O ₃ −0.3 · B ₂ O ₃ −0.1 · SiO ₂
Hole diameter of second gas ejection hole 12: 0.3 mm
Hole diameter of the first gas ejection hole 11: 0.1 mm
Position of first gas ejection hole 11: 1.2 times the diameter of glass melt 2 Diameter of glass melt 2: 8.35 mm
Number of second gas ejection holes 12: 350
Number of first gas ejection holes 11: 30
Heating temperature: 1850 ° C
Gas: Nitrogen gas

(Example 2)
A manufacturing process similar to that in Example 1 was performed except that the following conditions were adopted. As a result, a glass material having a diameter of 8.51 mm was obtained.

Glass composition (molar ratio): 0.6 · Tb ₂ O ₃ −0.3 · B ₂ O ₃ −0.1 · SiO ₂
Hole diameter of second gas ejection hole 12: 0.5 mm
Hole diameter of the first gas ejection hole 11: 0.4 mm
Position of first gas ejection hole 11: 1.1 times the diameter of glass melt Diameter of glass melt 2: 8.55 mm
Number of second gas ejection holes 12: 185
Number of first gas ejection holes 11: 15
Heating temperature: 1850 ° C
Gas: Nitrogen gas

(Example 3)
A manufacturing process similar to that in Example 1 was performed except that the following conditions were adopted. As a result, a glass material having a diameter of 9.23 mm was obtained.

Glass composition (molar ratio): 0.6 · Tb ₂ O ₃ −0.3 · B ₂ O ₃ −0.1 · SiO ₂
Hole diameter of second gas ejection hole 12: 0.5 mm
Hole diameter of the first gas ejection hole 11: 0.3 mm
Position of the first gas ejection hole 11: 1.0 times the diameter of the glass melt Diameter of the glass melt 2: 9.30 mm
Number of second gas ejection holes 12: 120
Number of first gas ejection holes 11: 32
Heating temperature: 1850 ° C
Gas: Nitrogen gas

(Comparative example)
A manufacturing process similar to that in Example 1 was performed except that the diameters of all the gas ejection holes were set to 0.3 mm. As a result, a glass material having a diameter up to 5.32 mm could be produced, but a glass material having a diameter of 6 mm or more could not be produced.

DESCRIPTION OF SYMBOLS 1 ... Glass raw material lump 2 ... Glass melt 2a ... Outer peripheral part 10 ... Forming member 10a ... Gas ejection part 10b ... Gas ejection surface 11 ... 1st gas ejection hole 12 ... 2nd gas ejection hole 20 ... Laser irradiation apparatus 21 ... Gas supply means 22 ... Gas

Claims (5)

In a state where the glass raw material lump is suspended in a substantially vertical direction, it is a method for producing a glass material by cooling after heating and melting,
In a state where the glass raw material lump is floated and melted, a plurality of first gas ejection holes located in the vicinity of the outer peripheral edge in the substantially horizontal direction of the melt of the glass raw material lump, and located inside the vicinity of the outer peripheral edge Preparing a molded member formed with a plurality of second gas ejection holes;
Arranging the glass raw material lump on the molded member;
A step of heating and melting the glass raw material lump in a suspended state by ejecting gas from the first gas ejection hole and the second gas ejection hole, and then cooling it,
The method for producing a glass material, wherein the gas ejected from the first gas ejection hole is ejected at a flow rate faster than the gas ejected from the second gas ejection hole. The manufacturing method of the glass material of Claim 1 with which the said 1st gas ejection hole is formed in the position 0.8 times-1.5 times the diameter of the substantially horizontal direction of the said melt. The manufacturing method of the glass material of Claim 1 or 2 with which the said 1st gas ejection hole is arranged circumferentially.   By making the diameter of the first gas ejection hole smaller than the diameter of the second gas ejection hole, the gas ejected from the first gas ejection hole is ejected from the second gas ejection hole. The method for producing a glass material according to any one of claims 1 to 3, wherein the glass material is ejected at a flow rate faster than gas. An apparatus for producing a glass material by cooling after heating and melting in a state where a glass raw material lump is suspended in a gas in a substantially vertical direction,
In a state where the glass raw material lump is floated and melted, a plurality of first gas ejection holes located in the vicinity of the outer peripheral edge in the substantially horizontal direction of the melt of the glass raw material lump, and located inside the vicinity of the outer peripheral edge A molded member formed with a plurality of second gas ejection holes,
A gas supply means for supplying gas to the first gas ejection hole and the second gas ejection hole; and a heating means for heating the glass raw material lump.
The glass material manufacturing apparatus, wherein a diameter of the first gas ejection hole is smaller than a diameter of the second gas ejection hole.

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