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WO2017179360A1 - Procédé et dispositif de fabrication de verre trempé - Google Patents

Procédé et dispositif de fabrication de verre trempé Download PDF

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Publication number
WO2017179360A1
WO2017179360A1 PCT/JP2017/010479 JP2017010479W WO2017179360A1 WO 2017179360 A1 WO2017179360 A1 WO 2017179360A1 JP 2017010479 W JP2017010479 W JP 2017010479W WO 2017179360 A1 WO2017179360 A1 WO 2017179360A1
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WO
WIPO (PCT)
Prior art keywords
glass
molten salt
film
tempered glass
ions
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2017/010479
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English (en)
Japanese (ja)
Inventor
田中　敦
睦 深田
清貴 木下
利之 梶岡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Electric Glass Co Ltd
Original Assignee
Nippon Electric Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Electric Glass Co Ltd filed Critical Nippon Electric Glass Co Ltd
Priority to JP2018511939A priority Critical patent/JP6827652B2/ja
Priority to CN201780005746.3A priority patent/CN108463443B/zh
Publication of WO2017179360A1 publication Critical patent/WO2017179360A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface

Definitions

  • the present invention relates to a method for producing tempered glass and an apparatus for producing tempered glass, and more specifically, relates to a method for producing tempered glass for chemically strengthening a glass plate by an ion exchange method and an apparatus for tempered glass.
  • a tempered glass plate that has been chemically strengthened as a cover glass has been used for touch panel displays mounted on electronic devices such as smartphones and tablet PCs.
  • Such a tempered glass plate is generally produced by chemically treating a glass plate containing an alkali metal as a composition with a tempering solution to form a compressive stress layer on the surface. Since such a tempered glass plate has a compressive stress layer on the main surface, the impact resistance to the main surface is improved. On the other hand, a tensile stress layer corresponding to the compressive stress layer on the main surface is formed inside such a tempered glass plate. If this tensile stress becomes excessively large, cracks on the end face are caused due to this. Damage due to progress (so-called self-destruction) is likely to occur. Further, when the compressive stress layer on the surface of the glass plate is formed to be shallow as a whole in order to reduce such tensile stress, there is a problem that sufficient impact resistance cannot be obtained at the end face.
  • Patent Document 1 by forming a film that suppresses ion exchange in advance on the main surface and suppressing the progress of chemical strengthening compared to the end surface, the compressive stress layer on the end surface is relatively deeper than the main surface.
  • a technique for forming and improving the strength at the end face is disclosed.
  • molten salt used for ion exchange of tempered glass gradually changes in liquid quality due to repeated use. Therefore, when a membrane that suppresses ion exchange is formed as in the technique of Cited Document 1, depending on the quality of the reinforcing liquid used for ion exchange, chemical strengthening is excessive at the location where the membrane that suppresses ion exchange is formed. In some cases, a sufficient compressive stress layer could not be obtained. That is, there is still room for improvement in the method for stably producing tempered glass having high strength.
  • the present invention has been made in view of such circumstances, and it is an object of the present invention to provide a tempered glass manufacturing method and a tempered glass manufacturing apparatus capable of stably manufacturing a tempered glass plate having high strength.
  • the method for producing tempered glass of the present invention is a method for producing tempered glass for exchanging ions on a glass surface layer, and a step of forming an ion permeation suppression film for suppressing ion permeation on at least a part of the surface of the glass
  • a step of bringing the molten salt into contact with the surface of the glass on which the ion permeation suppressing film is formed and exchanging ions, and the molten salt is mixed with water to form an aqueous solution having a molten salt concentration of 20% by mass.
  • the pH is 6.5 or more.
  • the molten salt preferably has a pH of 6.7 to 10 when mixed with water to obtain an aqueous solution having a molten salt concentration of 20% by mass. .
  • the method for producing tempered glass of the present invention preferably further comprises a step of adjusting the pH value when an aqueous solution is prepared by adding a basic substance to the molten salt.
  • the ions on the glass surface layer are sodium ions
  • the molten salt contains potassium ions
  • the basic substance contains potassium hydroxide.
  • the glass has a glass composition of mass%, SiO 2 45 to 75%, Al 2 O 3 1 to 30%, Na 2 O 0 to 20%, K 2 O 0 to 20%. %, And an ion permeation suppressing film is formed only on the main surface of the glass, and the formed glass is immersed in a molten salt at 370 to 480 ° C. for 0.1 to 72 hours for ion exchange. It is preferable.
  • the ion permeation suppression film preferably contains SiO 2 as a main component.
  • the method for producing tempered glass of the present invention further includes a step of adjusting the pH value of the aqueous solution by controlling the temperature of the molten salt.
  • the tempered glass manufacturing apparatus of the present invention is a tempered glass manufacturing apparatus provided with a salt bath containing molten salt for exchanging ions on the glass surface layer, and the molten salt is mixed with water so that the concentration of the molten salt is The pH when the aqueous solution is 20% by mass is 6.5 or more.
  • the tempered glass manufacturing apparatus of the present invention further includes a film forming apparatus that forms an ion permeation suppressing film that suppresses permeation of ions on at least a part of the surface of the glass, and a support apparatus that supports the formed glass.
  • the support device is preferably configured to be dipped in a salt bath while supporting the glass.
  • the present invention by appropriately adjusting the molten salt used for the chemical strengthening of glass, ion exchange is not excessively suppressed at the location where the ion permeation suppression film is formed, and the tempered glass plate has high strength. Can be manufactured stably.
  • FIG. 1A shows an example of a method for producing tempered glass of the present invention.
  • FIG. 1B shows an example of a method for producing the tempered glass of the present invention.
  • FIG. 1C shows an example of a method for producing the tempered glass of the present invention.
  • FIG. 1D shows an example of a method for producing the tempered glass of the present invention.
  • FIG. 2 is a flowchart showing another example of the method for producing tempered glass according to the present invention.
  • FIG. 1 is a diagram showing an example of a method for producing tempered glass of the present invention.
  • the preparation process is a process of preparing the original glass G1.
  • the original glass G1 is a glass that can be tempered using an ion exchange method.
  • the original glass G1 preferably contains, by mass%, SiO 2 45 to 75%, Al 2 O 3 1 to 30%, Na 2 O 0 to 20%, K 2 O 0 to 20% as a glass composition. If the glass composition range is regulated as described above, it becomes easy to achieve both ion exchange performance and devitrification resistance at a high level.
  • the thickness of the original glass G1 is, for example, 1.5 mm or less, preferably 1.3 mm or less, 1.1 mm or less, 1.0 mm or less, 0.8 mm or less, 0.7 mm or less, 0.6 mm or less, 0.5 mm or less, 0.4 mm or less, 0.3 mm or less, 0.2 mm or less, especially 0 mm. 1 mm or less.
  • the thickness of the original glass G1 is preferably 0.01 mm or more.
  • the dimensions of the main surface of the original glass G1 are, for example, 480 ⁇ 320 mm to 3350 ⁇ 3950 mm.
  • the original glass G1 is preferably formed using an overflow downdraw method, and its main surface S is not polished. With the original glass G1 thus formed, a tempered glass plate having high surface quality can be obtained at low cost. In addition, you may select arbitrarily the shaping
  • the original glass G1 may be formed using a float process, and the main surface S and the end surface E may be polished.
  • the film forming step is a step of forming the glass with film G2 by forming the ion permeation suppressing film M on at least a part of the surface of the original glass G1.
  • the ion permeation suppression film M is a film layer that suppresses permeation of ions when ion exchange is performed on the surface layer of the original glass G1 in the strengthening process described later.
  • the film-coated glass G2 has the ion permeation suppression film M formed only on the front and back main surfaces S, and the end face E is exposed.
  • the ion permeation suppression film M As a material of the ion permeation suppression film M, any material may be used as long as permeation of ions to be ion-exchanged can be suppressed.
  • the exchanged ions are alkali metal ions
  • the ion permeation suppression film M is, for example, a metal oxide, metal nitride, metal carbide, metal oxynitride, metal oxycarbide, metal carbonitride film, or the like. Is preferred.
  • the material of the ion permeation suppressive film M for example, SiO 2, Al 2 O 3 , SiN, SiC, Al 2 O 3, AlN, ZrO 2, TiO 2, Ta 2 O 5, Nb 2 O 5 , a film containing one or more of HfO 2 and SnO 2 .
  • the ion permeation suppression film M it is preferable to use SiO 2 as the main component of the ion permeation suppression film M because the ion permeation suppression film M can be easily formed at low cost and can function as an antireflection film.
  • Ion permeation suppressive film M is good as a film made of only SiO 2.
  • the ion permeation suppression film M may have a composition containing 99% or more of SiO 2 by mass%.
  • the thickness of the ion permeation suppression film M is preferably 5 to 300 nm, more preferably 20 to 200 nm, still more preferably 20 to 150 nm, 40 to 120 nm, and most preferably 80 to 100 nm.
  • the film formation method of the ion permeation suppression film M is a PVD method (physical vapor deposition method) such as a sputtering method or a vacuum evaporation method, a CVD method (chemical vapor deposition method) such as a thermal CVD method or a plasma CVD method, dip coating, etc.
  • a wet coating method such as a method or a slit coating method can be used.
  • a sputtering method and a dip coating method are preferable.
  • the deposition location of the ion permeation suppression film M may be set by any method.
  • the film formation may be performed in a state where a mask is previously applied to a non-film formation portion (end surface E in the present embodiment).
  • the tempering step is a step of chemically strengthening the film-coated glass G2 by an ion exchange method to obtain a film-coated tempered glass G3. Specifically, ion exchange is performed by immersing the film-coated glass G2 in a molten salt T containing alkali metal ions.
  • the pH value of the aqueous solution (hereinafter referred to as pH at the time of aqueous solution) is 6. It is a salt of 5 or more.
  • the aqueous pH is preferably 6.7 to 10, more preferably 6.8 to 8.5, and still more preferably 7.0 to 8.0.
  • the pH when water is in the range of 7.0 to 8.0.
  • the pH at the time of aqueous solution can be measured, for example, by once cooling and solidifying the molten salt, pulverizing and weighing the molten salt to prepare the aqueous solution.
  • the molten salt T in the present embodiment is, for example, potassium nitrate molten salt, but a well-known molten salt used for ion exchange of glass may be used.
  • the adjustment step of adjusting the pH of the molten salt T when it is in water within the above range before or after the strengthening step.
  • the pH at the time of aqueous solution can be adjusted by adding an additive to the molten salt T.
  • the additive is, for example, a basic substance.
  • the basic substance is a substance having a hydrogen ion index (pH) of more than 7 when mixed with water.
  • KOH, NaOH or the like can be used alone or in combination.
  • the temperature of the molten salt in the strengthening step may be arbitrarily determined, and is, for example, 350 to 500 ° C., preferably 370 to 480 ° C.
  • the time for immersing the film-coated glass G2 in the molten salt T may be arbitrarily determined, and is, for example, 0.1 to 72 hours, preferably 0.5 to 24 hours.
  • the tempering step sodium ions on the surface of the film-coated glass G2 and potassium ions in the molten salt T are exchanged to obtain a film-reinforced glass G3 having a compressive stress layer C on the surface.
  • a portion (main surface S) where the ion permeation suppression film M is provided is suppressed in ion exchange compared to the exposed portion E where the surface of the original glass G1 is exposed.
  • the depth of the compressive stress layer is reduced. In other words, in the exposed portion E, the ion exchange can proceed more easily than the portion where the ion permeation suppression film M is provided, and the depth of the compressive stress layer is increased.
  • the tempered glass with film G3 has a deeper compressive stress layer at the end surface than the main surface, and therefore has a lower internal tensile stress than the tempered glass strengthened entirely, and at the end portion. High impact resistance. Therefore, the damage resulting from the progress of the crack from the end can be suitably suppressed.
  • the ion permeation suppression film M when the above-described inorganic composition material is adopted as the ion permeation suppression film M, it is melted as compared with a conventional organic protective film or the like even when immersed in the molten salt T with the film provided. It is difficult to deteriorate the salt T.
  • the processing conditions such as the processing temperature and the dipping time in the tempering step may be appropriately determined according to the characteristics required for the tempered glass with film G3.
  • the processing conditions are preferably adjusted so that the depth of the compressive stress layer on the main surface S of the tempered glass G3 with film is smaller than the depth of the compressive stress layer on the exposed portion E.
  • the tempered glass G3 with a film can be used as a product as it is, but the ion permeation suppression film M can be used depending on the application. It may be peeled off. In the peeling step shown in FIG. 1D, the ion permeation suppression film M is peeled from the tempered glass G3 with film to obtain a tempered glass plate G4.
  • the ion permeation suppression film M is removed by attaching an etching solution to the tempered glass with film G3.
  • the ion permeation suppression film M is a film containing SiO 2
  • a solution containing fluorine, TMAH, EDP, KOH, or the like can be used as an etchant, and a hydrofluoric acid solution is particularly preferably used as an etchant.
  • the peeling method of the ion permeation suppression film M is not limited to the above, and a known method may be used as a method for removing the film provided on the glass plate.
  • the ion permeation suppression film M may be formed by machining such as polishing. It may be removed.
  • the peeling step only the ion permeation suppression film M on one main surface side may be removed, or the ion permeation suppression films M on both main surfaces may be removed. Further, the ion permeation suppression film M may be partially removed from each main surface, or the ion permeation suppression film M may be entirely removed.
  • the etching liquid is partially adhered using a spray, roll, brush, etc., or the masked tempered glass G3 is partially masked to etch the liquid. It is possible to remove the film by immersing the film in the film.
  • the entire tempered glass with film G3 may be immersed in an etching solution. If the entire tempered glass with film G3 is immersed in the etching solution in this way, there are cases where a tempered glass plate G4 with further improved strength can be obtained by reducing microcracks that cause damage.
  • the tempered glass G3 and the tempered glass G4 with less damage from the end face can be efficiently produced.
  • the material of the ion permeation suppression film M described above is an example, and any material may be used as long as the film can suppress permeation of ions exchanged in the strengthening process.
  • a processing step for performing any one of cutting, end surface processing, and drilling processing may be provided.
  • the glass plate may be appropriately washed and dried.
  • the manufacturing method of the tempered glass mentioned above can be implemented using the tempered glass manufacturing apparatus provided with the salt bath X which accommodated the said molten salt T.
  • the salt tub X is, for example, a tank made of a metal casing having an upper opening, and has an internal space filled with the molten salt T.
  • the said tempered glass manufacturing apparatus is further provided with the support apparatus (not shown) which is comprised by the shape and dimension which can be accommodated in the salt tub X, and can support the glass G2 with a film
  • the support device is a jig constituted by a metal frame such as stainless steel, for example.
  • the treatment of the strengthening step can be performed.
  • the tempered glass manufacturing apparatus may further include a film forming apparatus (not shown) that performs the film forming process.
  • a film forming apparatus a known sputter film forming apparatus or the like can be used.
  • FIG. 2 is a flowchart showing another example of the method for producing tempered glass according to the present invention.
  • the method includes a preparation step S1, a film formation step S2, a molten salt generation step S3, a pH measurement step S4, a determination step S5, a pH adjustment step S6, a strengthening step S7, and a peeling step S8.
  • the preparation step S1, the film formation step S2, and the peeling step S8 are the same as the example in FIG.
  • Generation process S3 is a process which heats and melts metal nitrate (for example, potassium nitrate etc.), and obtains molten salt T.
  • metal nitrate for example, potassium nitrate etc.
  • PH measurement step S4 is performed after the molten salt generation step S3.
  • the pH measurement step S4 the pH when the molten salt T is mixed with water to make an aqueous solution having a concentration of 20% by mass is measured.
  • an off-the-shelf pH meter is used for measuring the pH.
  • the determination step S5 it is determined whether or not the pH value of the molten salt T measured in the pH measurement step S4 is suitable for the strengthening step S7. This determination is made by comparison with a predetermined reference value.
  • the reference value is set according to various conditions such as dimensions, thickness, DOL, and CS of the tempered glass. For example, when the reference value of pH is 6.5, when the measured pH value of the molten salt T is 6.5 or more (Yes in determination step S5), the process proceeds to the next strengthening step S7. When the measured pH value of the molten salt T is less than 6.5 (No in the determination step S5), the pH adjustment step S6 is performed before the strengthening step S7.
  • the pH adjustment step S6 at least one step such as a step of adding a basic substance to the molten salt T, a step of immersing the film-adjusting member for pH adjustment in the molten salt T, or a step of controlling the temperature of the molten salt T. To adjust the pH value of the molten salt T.
  • a basic substance having a pH higher than 7 when mixed with water is added to the molten salt T, and the molten salt T Adjust the pH.
  • the membrane-attached member In the step of immersing the membrane-attached member for pH adjustment in the molten salt, the membrane-attached member is immersed in the molten salt T, and the membrane-attached member is melted when the pH of the molten salt T reaches a desired value.
  • pH membrane with members for adjustment for example, be constituted by a glass substrate having a film made of SiO 2 is desired, it may be used after forming the SiO 2 film on the metal substrate.
  • the pH value can be lowered. That is, the hydroxide ions in the molten salt T break Si—O bonds in the SiO 2 film.
  • the SiO 2 film is desirably formed on a glass or metal substrate by sputtering, but is not limited thereto, and may be formed by wet coating or spin coating.
  • the pH value of the molten salt T can be increased by maintaining the molten salt T at a temperature equal to or higher than its boiling point.
  • a part of the potassium nitrate is changed to potassium nitrite. Since this potassium nitrite has deliquescence, moisture (H 2 O) in the atmosphere is taken into the molten salt T.
  • the film-coated glass G2 is immersed in the molten salt T accommodated in the salt bath X, as in the example of FIG. After immersion for a certain time, the tempered glass with film G3 is taken out from the salt bath X. The tempered glass with film G3 becomes the tempered glass plate G4 after the peeling step S8.
  • this invention is not limited to the structure of the said embodiment, It is not limited to the above-mentioned effect.
  • the present invention can be variously modified without departing from the gist of the present invention.
  • the present invention is not limited to this, and the pH adjusting step S6 and the tempering step S7 may be executed simultaneously.
  • the pH adjusting step S6 may be executed simultaneously.
  • the tempered glass with film G3 may be reinforced by immersing the molten salt T in the molten salt T while maintaining the molten salt T at a temperature equal to or higher than the boiling point.
  • the pH value of the molten salt T may change greatly during strengthening.
  • the salt bath X be made of quartz. According to this, since hydrogen ions do not come out of the molten salt T, a change in pH value can be suppressed as compared with the metal salt bath X.
  • the glass composition is glass so that it contains 61.6% of SiO 2 , 19.6% of Al 2 O 3 , 0.8% of B 2 O 3 , 16% of Na 2 O, and 2 % of K 2 O in mass%.
  • the raw materials were mixed and melted, and molded using an overflow downdraw method to obtain a plurality of original glasses having a thickness of 0.4 mm.
  • membrane which has an exposed part in an end surface was obtained by cutting out into the rectangular shape of a dimension.
  • the samples No. 10 to 18 were cut as described above without performing the film formation.
  • the obtained glass with a film was immersed in a 430 ° C. potassium nitrate solution having a pH at the time of water listed in Table 1 for 5 hours to chemically strengthen, washed with pure water and naturally dried, and then No. 1 in Table 1. 1 to 18 tempered glass plate samples were obtained.
  • Main surface compressive stress value CS, main surface stress depth DOL, and internal tensile stress CT were measured with a stress meter (FSM-6000LE and FsmXP manufactured by Orihara Seisakusho).
  • the falling ball test was carried out by placing the edge of a tempered glass plate sample having a size of 65 mm in length and 130 mm in width created in the same manner as described above on a frame-shaped jig having an open center portion made of paper bakelite.
  • a steel ball was dropped on the center of the glass, and the height at which it was damaged by a single collision was recorded. Specifically, from a height of 15 cm, a steel ball is dropped in increments of 5 cm, the height at which the tempered glass is broken is recorded, the height at which the tempered glass is broken is Weibull plotted, and the height at which the breakage probability has reached 63% is recorded. Obtained as an average value.
  • Sample No. 9 which is a comparative example, has a pH under water that is smaller than 6.5. Therefore, ion exchange is excessively suppressed by the ion permeation suppression membrane, and the surface compressive stress value CS and The surface compressive stress depth DOL could not be obtained.
  • a compressive stress layer having an appropriate surface compressive stress value and surface compressive stress depth was formed on the surface on which the ion permeation suppression film was formed.
  • each sample of the example was prepared by strengthening with an ion permeation suppression film formed on the main surface and an exposed portion on the end surface, and therefore compression of the surface and end surface
  • the balance of stress is suitably set, and as a result, the internal tensile stress CT is reduced as compared with the samples of Comparative Examples No. 10 to 18 which are not formed with an ion permeation suppression film and are strengthened with pH under water conditions under the same conditions. It is harder to self-destruct.
  • Table 3 below shows the change of the pH of the molten salt with respect to the immersion time when the glass plate on which the SiO 2 film is formed is immersed in molten potassium nitrate held at a predetermined temperature (temperature below the boiling point). Show. Sample No. shown in Table 3
  • Each of the molten salts 21 to 24 contains 600 g of potassium nitrate and 13.6 g of sodium nitrate. Furthermore, sample no. The 21 molten salt contains 0.10 g of potassium hydroxide. Sample No. The 22 molten salt contains 0.60 g of potassium hydroxide. Sample No. The molten salt of No. 23 was obtained by adding 6.00 g of potassium hydroxide to Sample No. The 24 molten salt contains 0.05 g of potassium hydroxide.
  • the pH value of the molten salt shown in Table 3 is a value when the molten salt is a 20% by mass aqueous solution. As shown in Table 3, each sample No. From 21 to 24, it was found that the pH value of the molten salt decreased with the passage of time. From this, it can be seen that the glass plate on which the SiO 2 film is formed can be effectively used as an adjusting material for lowering the pH value of the molten salt in the pH adjusting step.
  • the present inventors conducted a test for confirming the influence of the salt bath containing the molten salt T on the pH of the molten salt.
  • the molten salt is accommodated in a quartz salt bath (beaker) and a stainless steel salt bath, and the pH value is measured when the molten salt is made into a 20% by mass aqueous solution after a certain period of time. did.
  • the molten salt contains 600 g of potassium nitrate.
  • the temperature of the molten salt was maintained below the boiling point.
  • Table 4 The test results are shown in Table 4 below. As shown in Table 4, the molten salt accommodated in the quartz salt tub has a smaller degree of change (increase) in pH with the passage of time than that accommodated in the stainless steel salt tub. I understand.
  • the present inventors conducted a test to confirm the relationship between temperature and pH change in molten salt.
  • the temperature of the potassium nitrate molten salt was set to 400 ° C., 430 ° C., and 460 ° C., and the pH value of the molten salt (20% by mass aqueous solution) after a lapse of a fixed time was measured.
  • the test results are shown in Table 5 below. As shown in Table 5, it can be seen that the higher the temperature of the molten salt, the greater the change (increase) in the pH of the molten salt with respect to the elapsed time. This test confirmed that the pH of the molten salt can be adjusted by controlling the temperature of the molten salt in the pH adjustment step.
  • the tempered glass plate of the present invention and the manufacturing method thereof are useful as a glass substrate used for a touch panel display and the like, a manufacturing method thereof, and the like.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Geochemistry & Mineralogy (AREA)
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  • Surface Treatment Of Glass (AREA)

Abstract

L'invention concerne un procédé qui permet de fabriquer un verre trempé par exécution d'un échange d'ions sur la couche de surface du verre et qui est caractérisé en ce qu'il comprend : une étape consistant à former, sur au moins une partie de la surface du verre, un film de suppression de la perméation d'ions qui supprime la perméation d'ions ; une étape consistant à mettre du sel fondu en contact avec la surface du verre sur laquelle le film de suppression de la perméation d'ions est formé et à exécuter un échange d'ions. Le sel fondu possède un pH supérieur ou égal à 6,5 lorsqu'il est mélangé avec de l'eau pour produire une solution aqueuse ayant une concentration de 20 % en masse.
PCT/JP2017/010479 2016-04-12 2017-03-15 Procédé et dispositif de fabrication de verre trempé Ceased WO2017179360A1 (fr)

Priority Applications (2)

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JP2018511939A JP6827652B2 (ja) 2016-04-12 2017-03-15 強化ガラスの製造方法および強化ガラス製造装置
CN201780005746.3A CN108463443B (zh) 2016-04-12 2017-03-15 强化玻璃的制造方法及强化玻璃制造装置

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JP2016079277 2016-04-12
JP2016-079277 2016-04-12

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CN (1) CN108463443B (fr)
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018062141A1 (fr) * 2016-09-30 2018-04-05 旭硝子株式会社 Procédé de production de verre trempé chimiquement
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US12426184B2 (en) 2019-08-29 2025-09-23 Corning Incorporated Foldable apparatus, ribbons, and methods of making
US12481316B2 (en) 2019-08-29 2025-11-25 Corning Incorporated Foldable apparatus, foldable substrate, and methods of making

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WO2024041455A1 (fr) * 2022-08-22 2024-02-29 福耀高性能玻璃科技(福建)有限公司 Verre à renforcer possédant un revêtement, ensemble de verre à renforcer et plaque de verre composite soudée au laser
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CN116768494A (zh) * 2019-04-26 2023-09-19 Ａｇｃ株式会社 熔融盐组合物的寿命延长方法、化学强化玻璃的制造方法、玻璃助剂和玻璃的原材料
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US12481316B2 (en) 2019-08-29 2025-11-25 Corning Incorporated Foldable apparatus, foldable substrate, and methods of making

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