US20160332909A1 - Apparatuses and methods for holding, retaining, and/or processing glassware articles - Google Patents
Apparatuses and methods for holding, retaining, and/or processing glassware articles Download PDFInfo
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- US20160332909A1 US20160332909A1 US15/151,168 US201615151168A US2016332909A1 US 20160332909 A1 US20160332909 A1 US 20160332909A1 US 201615151168 A US201615151168 A US 201615151168A US 2016332909 A1 US2016332909 A1 US 2016332909A1
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- US
- United States
- Prior art keywords
- glassware
- cover plate
- bottom support
- support floor
- securing member
- 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.)
- Abandoned
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B11/00—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto
- B08B11/02—Devices for holding articles during cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/20—Cleaning containers, e.g. tanks by using apparatus into or on to which containers, e.g. bottles, jars, cans are brought
- B08B9/42—Cleaning containers, e.g. tanks by using apparatus into or on to which containers, e.g. bottles, jars, cans are brought the apparatus being characterised by means for conveying or carrying containers therethrough
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
Definitions
- glass breakage is a concern, particularly in the packaging of food, beverages, and pharmaceuticals. Breakage can be costly in the food, beverage, and pharmaceutical packaging industries because, for example, breakage within a filling line may require that neighboring unbroken containers be discarded as the containers may contain fragments from the broken container. Breakage may also require that the filling line be slowed or stopped, lowering production yields. Further, non-catastrophic breakage (i.e., when the glass cracks but does not break) may cause the contents of the glass package or container to lose their sterility which, in turn, may result in costly product recalls.
- FIG. 11 schematically depicts the process described in the flow diagram of FIG. 10 , according to one or more embodiments shown and described herein;
- the bottom support floor 500 may be substantially identical to the cover plate 400 .
- the magazine apparatus 100 may be stacked with another magazine apparatus 100 so that the bottom support floor 500 of a top magazine apparatus 100 serves as the cover plate 400 for a bottom magazine apparatus 100 .
- the ion-exchange tank 614 contains a bath of molten salt 616 , such as a molten alkali salt, such as KNO 3 , NaNO 3 and/or combinations thereof.
- the bath of molten salt is 100% molten KNO 3 which is maintained at a temperature greater than or equal to about 350° C. and less than or equal to about 500° C.
- baths of molten alkali salt having various other compositions and/or temperatures may also be used to facilitate ion-exchange of the glass articles.
- the molten salt 616 should be held at a temperature as high as is possible given process constraints. Without being bound by theory, it is believed that a higher salt bath temperature may reduce the ratio of salt density to viscosity.
Abstract
According to embodiments disclosed herein, an apparatus may hold and retain glass articles during processing. The apparatus may define a plurality of receiving volumes for holding glass articles. The apparatus may include a bottom support floor, a glassware-securing member positioned above the bottom support floor, and a cover plate positioned above the glassware-securing member. The bottom support floor may include a plurality of fluid passages, the glassware-securing member may include a plurality of glassware-retaining openings, and the cover plate may include a plurality of fluid passages.
Description
- The present application claims priority to U.S. Provisional Application No. 62/159,653 filed May 11, 2015 entitled, “Apparatuses and Methods for Holding, Retaining, and/or Processing Glassware Articles,” the entirety of which is incorporated by reference herein.
- 1. Field
- The present specification generally relates to magazine apparatuses for holding and retaining glass articles during processing and, more specifically, to magazine apparatuses for holding and retaining glass articles during ion-exchange processing.
- 2. Technical Background
- Historically, glass has been used as a preferred material for many applications, including food and beverage packaging, pharmaceutical packaging, kitchen and laboratory glassware, and windows or other architectural features, because of its hermeticity, optical clarity, and excellent chemical durability relative to other materials.
- However, use of glass for many applications is limited by the mechanical performance of the glass. In particular, glass breakage is a concern, particularly in the packaging of food, beverages, and pharmaceuticals. Breakage can be costly in the food, beverage, and pharmaceutical packaging industries because, for example, breakage within a filling line may require that neighboring unbroken containers be discarded as the containers may contain fragments from the broken container. Breakage may also require that the filling line be slowed or stopped, lowering production yields. Further, non-catastrophic breakage (i.e., when the glass cracks but does not break) may cause the contents of the glass package or container to lose their sterility which, in turn, may result in costly product recalls.
- One root cause of glass breakage is the introduction of flaws in the surface of the glass as the glass is processed and/or during subsequent filling. These flaws may be introduced in the surface of the glass from a variety of sources including contact between adjacent pieces of glassware and contact between the glassware and equipment, such as handling and/or filling equipment. Regardless of the source, the presence of these flaws may ultimately lead to glass breakage.
- Additionally, ion-exchanged glass, sometimes referred to as chemically strengthened glass, may provide additional strength. However, both the exterior portion and the interior portion of a glass container must be contacted with an ion-exchange bath to balance the stresses imparted to the glass. Suitably securing glass containers to allow for complete submersion in an ion-exchange bath while not introducing flaws on the surface of the glass is difficult.
- Accordingly, a need exists for alternative apparatuses for holding glass articles during processing to mitigate glass breakage while allowing for full contact of the interior and exterior regions of glass articles with processing baths, such as ion-exchange baths.
- According to one embodiment, an apparatus may hold and retain glass articles during processing. The apparatus may define a plurality of receiving volumes for holding glass articles. The apparatus may comprise a bottom support floor, a glassware-securing member positioned above the bottom support floor, and a cover plate positioned above the glassware-securing member. The bottom support floor may comprise a plurality of fluid passages, the glassware-securing member may comprise a plurality of glassware-retaining openings, and the cover plate may comprise a plurality of fluid passages. Each of the bottom support floor, the glassware-securing member, and the cover plate may be substantially planar. The bottom support floor, the glassware-securing member, and the cover plate may be substantially parallel with one another. Each glassware-retaining opening of the glassware-securing member may define a width dimension of the receiving volume. The bottom support floor and the cover plate may define a height dimension of the receiving volume.
- In another embodiment, an assembly may hold and retain glass articles during processing. The assembly may comprise a plurality of magazine apparatuses, and one or more of the magazine apparatuses may define a plurality of receiving volumes. One or more of the magazine apparatuses may comprise a bottom support floor, a glassware-securing member positioned above the bottom support floor, and a cover plate positioned above the glassware-securing member. The bottom support floor may comprise a plurality of fluid passages, the glassware-securing member may comprise a plurality of glassware-retaining openings, and the cover plate may comprise a plurality of fluid passages. Each of the bottom support floor, the glassware-securing member, and the cover plate may be substantially planar. The bottom support floor, the glassware-securing member, and the cover plate may be substantially parallel with one another. Each glassware-retaining opening of the glassware-securing member may define a width dimension of the receiving volume. The bottom support floor and cover plate may define a height dimension of the receiving volume.
- In yet another embodiment, a method for ion-exchanging glass articles may comprise supplying an apparatus or assembly for holding and retaining glass articles during processing, positioning one or more glass articles one or more of the receiving volumes of the apparatus or assembly, and at least partially submerging the apparatus or assembly in an ion-exchange bath to contact the one or more glass articles with the ion-exchange bath.
- Additional features and advantages of the apparatuses described herein will be set forth in the detailed description which follows, and in part will be readily apparent to those skilled in the art from that description or recognized by practicing the embodiments described herein, including the detailed description which follows, the claims, as well as the appended drawings.
- It is to be understood that both the foregoing general description and the following detailed description describe various embodiments and are intended to provide an overview or framework for understanding the nature and character of the claimed subject matter. The accompanying drawings are included to provide a further understanding of the various embodiments, and are incorporated into and constitute a part of this specification. The drawings illustrate the various embodiments described herein, and together with the description serve to explain the principles and operations of the claimed subject matter.
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FIG. 1 schematically depicts a perspective view of a magazine apparatus without a cover plate, according to one or more embodiments shown and described herein; -
FIG. 2 schematically depicts a perspective view of a magazine apparatus with a cover plate, according to one or more embodiments shown and described herein; -
FIG. 3 schematically depicts an exploded view of a magazine apparatus, according to one or more embodiments shown and described herein; -
FIG. 4 schematically depicts a cross-sectional view of a glass article, according to one or more embodiments shown and described herein; -
FIG. 5 schematically depicts an enlarged perspective view of a magazine apparatus without a cover plate, according to one or more embodiments shown and described herein; -
FIG. 6 schematically depicts the bottom support floor ofFIG. 5 , according to one or more embodiments shown and described herein; -
FIG. 7 schematically depicts an enlarged perspective view of a magazine apparatus without a cover plate, according to one or more embodiments shown and described herein; -
FIG. 8 schematically depicts the bottom support floor ofFIG. 7 , according to one or more embodiments shown and described herein; -
FIG. 9 schematically depict a cross-sectional view of a loaded cassette assembly, according to one or more embodiments shown and described herein; -
FIG. 10 depicts a process flow diagram of a method for strengthening glass articles by ion-exchange, according to one or more embodiments shown and described herein; -
FIG. 11 schematically depicts the process described in the flow diagram ofFIG. 10 , according to one or more embodiments shown and described herein; -
FIG. 12 schematically depicts a glass article at a non-normal angel, according to one or more embodiments shown and described herein; -
FIG. 13 shows test data for vial filling, according to one or more embodiments shown and described herein. - Reference will now be made in detail to embodiments of magazine apparatuses for holding and retaining glass articles during processing, examples of which are illustrated in the accompanying drawings. Whenever possible, the same reference numerals will be used throughout the drawings to refer to the same or like parts. One embodiment of an apparatus for holding and retaining glass articles during processing is schematically depicted in
FIG. 1 . The magazine apparatus generally comprises a plurality of receiving volumes, where each receiving volume can hold and retain a glass article, such as a vial. The magazine apparatus may be suitable to securely hold the glass articles as they are submerged in an ion-exchange salt bath. For example, in one embodiment, glass articles may be secured in the magazine apparatus and the magazine apparatus may be submerged in an ion-exchange bath in a process which chemically strengthens the glass articles. In some embodiments, several magazine apparatuses may be coupled with one another in an assembly, and the assembly may be submerged in the ion-exchange bath. Generally, the magazine apparatuses may be suitable to be manipulated such that the glass articles may be submerged into the ion-exchange bath at an angle non-normal relative to the surface of the bath. - The magazine apparatuses described herein may be suitable to hold and retain glass articles, such as glass containers with a wide variety of geometries. As used herein, “glass article” may refer to any glassware, such as, but not limited to glass formed in the shape of a vial, ampoule, ampul, bottle, flask, phial, beaker, bucket, carafe, vat, syringe body, cartridge or the like. Additionally, “glass articles” may be referred to herein as “glassware” and these terms may be interchangeable. Various embodiments of apparatuses for holding and retaining glass articles during processing will be described in further detail herein with specific reference to the appended drawings.
- As noted herein, the breakage of glass articles during processing and/or filling is a source of product loss and may lead to process inefficiencies and increased costs. Additionally, cosmetic flaws in glass articles are often undesirable to users. Strengthening of glass articles can assist in mitigating breakage and scratching. Glass articles can be strengthened using a variety of techniques, including chemical and thermal tempering. For example, chemical tempering, sometimes called ion-exchange strengthening, can be used to strengthen glass articles through the introduction of a layer of compressive stress in the surface of the glass articles. The compressive stress is introduced by submerging the glass article in a molten salt bath, sometimes referred to as an ion-exchange bath. As ions from the glass are replaced by relatively larger ions from the molten salt, a compressive stress is induced in the surface of the glass. During chemical tempering, glass articles, such as glass containers, may be mechanically manipulated to both fill and empty the glass articles of molten salt.
- While chemical tempering improves the strength of the glass articles, mechanical manipulation of the glass articles during the strengthening process may introduce flaws in the surface of the glass. For example, contact between the glass articles and the fixturing, such as a magazine apparatus, used to retain the glass articles during processing, may introduce flaws in the glass, particularly when the glass articles and the fixturing are initially submerged in the molten salt bath and/or when the fixturing and glass articles are withdrawn from the molten salt bath and rotated to empty the glass articles of molten salt. Specifically, as a glass article is submerged it may be buoyant and thus be propelled upward relative to the fixturing. Moreover, after the ion-exchange process is complete, the fixturing and glass articles are withdrawn from the molten salt bath and the fixturing is rotated to empty the glass articles of molten salt contained within the interior volume of the glass articles. As the fixturing is rotated, the glass articles may abruptly collide with the fixturing. This blunt force impact between the glass articles and the fixturing may introduce flaws in the surface of the glass.
- In most cases the flaws are superficial and are contained within the layer of surface compressive stress induced in the glass. This surface compressive stress prevents the flaws from growing into cracks. However, in some cases, the flaws may extend through the layer of surface compressive stress which may lead to breakage of the glass articles.
- The magazine apparatuses for holding and retaining glass articles during processing described herein mitigate the introduction of flaws in the glass articles retained therein. Additionally, the magazine apparatuses described herein allow for acceptable levels of fluid contact by the molten salt bath with all areas (interior and exterior) of the glass article when the magazine apparatus is partially or fully submerged in the molten salt bath. Referring now to
FIGS. 1, 2 and 3 , one embodiment of amagazine apparatus 100 for holding and retainingglass articles 900 during processing is schematically depicted. Themagazine apparatus 100 generally includes abottom support floor 500, a plurality of glassware-securingmembers 200, and acover plate 400. Specifically,FIG. 1 shows amagazine apparatus 100 which does not have an attachedcover plate 400, andFIG. 2 shows amagazine apparatus 100 with an attachedcover plate 400.FIG. 3 shows an exploded view of thebottom support floor 500, the glassware-securingmembers 200, and thecover plate 400. When themagazine apparatus 100 does not have an attachedcover plate 400,glass articles 900 may be freely moved into and out of themagazine apparatus 100. However, when thecover plate 400 of themagazine apparatus 100 is positioned over the glassware-securingmembers 200,glass articles 900 positioned in themagazine apparatus 100 are retained as themagazine apparatus 100 is manipulated and maneuvered, including when themagazine apparatus 100 is rotated about a horizontal axis to facilitate emptying theglass articles 900 of a processing fluid. In other embodiments, themagazine apparatus 100 may not have an attachedcover plate 400, and may instead utilize another section of an adjacently stacked magazine apparatus, such as the bottom support floor of a magazine apparatus stacked above themagazine apparatus 100, as itscover plate 400. It should be understood that, as used herein, acover plate 400 may be a separate structure that is attached to thebottom support floor 500 and/or glassware-securingmembers 200 or may be a portion of anothermagazine apparatus 100. - In one embodiment, the components of the
magazine apparatus 100 may be shaped and sized to securely holdglass articles 900 shaped as vials. As shown inFIG. 4 , theglass articles 900 may generally include abody section 902, aneck section 904 above thebody section 902, and anopening 906 leading through the neck and connected to theinterior volume 910. Thebody section 902 substantially surrounds theinterior volume 910 of theglass articles 900 with abottom section 914 andside walls 916. Theneck section 904 generally connects thebody section 902 with theopening 906. Theopening 906 may be surrounded by acollar 908 extending outward from the top of theneck section 904 of theglass article 900. Thebody section 902 may have a curvedbottom edge 918 and acurved area 912 adjacent theneck section 904. Generally, theneck section 904,body section 902, andcollar 908 may have a generally circular-shaped cross section, each comprising an exterior diameter. In one embodiment, the diameter of the collar (da inFIG. 4 ) is greater than the diameter of the neck section (dn inFIG. 4 ) and the diameter of the body section (db inFIG. 4 ) is greater than the diameter of the collar, da. Additionally, theopening 906 comprises a diameter (dm inFIG. 4 ), referred to sometimes herein as the diameter of the mouth, which is less than the diameter of the neck (dn). Eachglass articles 900 may have a major axis (in the Z-direction inFIG. 4 ) which may be normal to the diameter of the body db and the diameter of the opening dm. - Generally, the
bottom support floor 500 may be substantially planar in shape, and theglass articles 900 rest upon thebottom support floor 500. As shown inFIG. 3 , thebottom support floor 500 is planar, and a length (i.e., the dimension in the X-direction) and width (i.e., the dimension in the Y-direction) of the bottom support floor are much greater than the height (i.e., in the Z-direction) of thebottom support floor 500. Thebottom support floor 500 may comprisefluid passages 510 to allow a processing fluid, such as the molten salt bath used in ion-exchange processing, to pass through thebottom support floor 500 and contact theglass articles 900 positioned in themagazine apparatus 100. In embodiments, thebottom support floor 500 may be formed from a rigid wire mesh, as depicted inFIGS. 1-3 . In other embodiments, thebottom support floor 500 may comprise a planar sheet formed with machined holes which a processing fluid, such as the molten salt bath used in ion-exchange processing, to pass through thebottom support floor 500 and contact theglass articles 900 positioned in themagazine apparatus 100. Alternatively, thebottom support floor 500 may be constructed with any generally planar geometry and with openings which allows for the passage of a fluid through thebottom support floor 500 while simultaneously supporting a plurality ofglass articles 900 resting thereon. Generally, thebottom support floor 500 may be any generally planar shaped article which will allow for the passage of fluid but does not allow for the passage ofglass articles 900. - Positioned above the
bottom support floor 500 are one or more glassware-securingmembers 200. As used herein, he terms “above” or “below” generally refer to the relative positioning of components in the Z-direction of the coordinates depicted inFIGS. 1-3 . The glassware-securingmembers 200 may be substantially planar in shape, and comprise a plurality of glassware-retainingopenings 210. As shown inFIG. 3 , the glassware-securingmembers 200 are substantially planar, and a length (i.e., in the dimension of the X-direction) and a width (i.e., in the dimension of the Y-direction) of the glassware-securingmember 200 are much greater than the height (i.e., in the dimension of the Z-direction) of the glassware-securingmember 200. WhileFIGS. 1-3 depict embodiments ofmagazine apparatuses 100 comprising two glassware-securingmembers 200, there can be any number of glassware-securingmembers 200 positioned between thebottom support floor 500 and thecover plate 400, such as one, three, four, five, six, or even more glassware-securing members. Multiple glassware-securingmembers 200 may be positioned in a generally parallel configuration. The number of glassware-securingmembers 200 may depend on the geometry of theglass articles 900 being retained. - Each glassware-securing
member 200 comprises glassware-retainingopenings 210 which at least partially define a receivingvolume 220 in which asingle glass article 900 can be received and secured. In one embodiment, the glassware-retainingopenings 210 of the glassware-securingmember 200 are approximately circularly shaped. Such an embodiment may be suitable for housing glass articles with circular exterior cross sections, such as those depicted inFIG. 4 . However, in other embodiments, the glassware-retainingopenings 210 may have geometries other than circular, such as triangular, rectangular, pentagonal, or other geometries suitable to securely houseglass articles 900 with cross-sectional geometries that are non-circular. The glassware-retainingopenings 210 may be slightly larger than the largest cross-sectional diameter of theglass articles 900 to be received and secured therein, shown in the embodiment ofFIG. 4 as db. - The glassware-retaining
openings 210 may be arranged in two dimensional arrays in the X-direction and Y-direction. For example, the glassware-retainingopenings 210 could be arranged in rows and columns, or could be arranged in other configurations such as the offset pattern shown inFIG. 1 . - In embodiments, a
cover plate 400 may be positioned above thebottom support floor 500 and glassware-securingmembers 200. Thecover plate 400 may be substantially planar in shape and comprise a plurality offluid passages 410. As shown inFIG. 3 , thecover plate 400 is substantially planar, and a length (i.e., in the dimension of the X-direction) and width (i.e., in the dimension of the Y-direction) of thecover plate 400 is much greater than the height (i.e., in the dimension of the Z-direction) of thecover plate 400. - The
cover plate 400 comprisesfluid passages 410 which allow for a processing fluid, such as the molten salt bath used in ion-exchange processing, to flow through thecover plate 400 and into the interior region of themagazine apparatus 100. In one embodiment, thefluid passages 410 of thecover plate 400 are approximately circularly shaped. Such an embodiment may be suitable forhousing glass articles 900 with circular mouth cross sections, such as those depicted inFIG. 4 . However, in other embodiments, thefluid passages 410 may have geometries other than circular. Thefluid passages 410 may be arranged in two dimensional arrays in the X-direction and Y-direction. For example, thefluid passages 410 could be arranged in rows and columns, or could be arranged in other configurations. - The
bottom support floor 500, the glassware-securingmembers 200, and thecover plate 400 may be substantially parallel relative to one another. Thebottom support floor 500, the glassware-retainingopenings 210 in the glassware-securingmembers 200, and thecover plate 400 define a plurality of receivingvolumes 220. Each receivingvolume 220 may securely house anindividual glass article 900. Thebottom support floor 500 and thecover plate 400 may define a height dimension of the receiving volume 220 (in the Z-direction). Thebottom support floor 500 and thecover plate 400 secure aglass article 900 in the vertical direction by restricting its movement in the vertical direction. Each glassware-retainingopening 210 of the glassware-securingmember 200 defines a width dimension (in the X-direction and Y-direction ofFIG. 1 ) of the receivingvolume 220. As such, the glassware-retainingopening 210 secures aglass article 900 by restricting its movement in the width direction (X-direction and Y-direction ofFIG. 1 ). Generally, theglass article 900 is positioned in a receiving volume where it major axis is in the height dimension. - The
magazine apparatus 100 may further comprisevertical supports 300 that securely connect thebottom support floor 500, the glassware-securingmembers 200, and may removably secure thecover plate 400. Thevertical supports 300 can be any mechanical fastening device suitable to connect thebottom support floor 500, the glassware-securingmembers 200, and/or thecover plate 400 with one another. In some embodiments, all or at least a portion of thevertical support 300 may comprise a unitary body. In one embodiment, one or more of thebottom support floor 500, the glassware-securingmembers 200, thecover plate 400, and thevertical support 300 may be formed as a unitary body. In other embodiments, one or more of thebottom support floor 500, the glassware-securingmembers 200, thecover plate 400, and thevertical support 300 may be secured together may mechanical means such as, but not limited to, screws, bolts, welding, glued, etc. Note thatFIG. 3 does not depictvertical supports 300. In one embodiment, thevertical supports 300 may allow for thecover plate 400 to be removably attached to the other sections of themagazine apparatus 100. -
FIGS. 5 and 7 depict embodiments of magazine apparatuses 100 (without cover plates) which havebottom support floors 500 with differing geometries.FIG. 5 shows amagazine apparatus 100 that includes abottom support floor 500 in a diagonal crisscrossing pattern (as depicted inFIG. 6 ).FIG. 7 shows amagazine apparatus 100 that includes abottom support floor 500 comprising a wire mesh geometry.FIGS. 6 and 8 show thebottom support floors 500 of themagazine apparatuses 100 depicted inFIGS. 5 and 7 , respectively. - In one embodiment, one or more of the
fluid passages 410 may be aligned with the glassware-retainingopenings 210. For example, eachfluid passage 410 may be positioned directly above a glassware-retainingopening 210, as is shown inFIGS. 1-3 . The diameter of eachfluid passage 410 may be less than the diameter of each glassware-retainingopening 210. In one embodiment, themagazine apparatus 100 may be designed to house glass articles similar or identical in geometry to the glass article depicted inFIG. 4 . The glassware-retainingopenings 210 may have a diameter slightly larger than the body (db) of theglass article 900. In some embodiments such as, but not limited to, embodiments where thefluid passages 410 are aligned with the glassware-retainingopenings 210, thefluid passages 410 may be smaller than the db of theglass articles 900. In one embodiment, the diameter of eachfluid passage 410 above a glassware-retainingopening 210 may be less than the diameter of each glassware-retainingopening 210. Eachfluid passage 410 may have a diameter that is larger than the diameter of the mouth dm and less than the diameter of the collar da of a housedglass article 900. In such a configuration, theopening 906 is not blocked by thecover plate 400 but theglass article 900 in constrained in movement because its collar diameter da is greater than the diameter of thefluid passage 410. - In another embodiment, a
single fluid passage 410 may aligned and shaped to allow for fluid passage into several receivingvolumes 220 defined by several glassware-retainingopenings 210. For example, thefluid passages 410 may be shaped as an elongated channels with ends shaped as semi-circles of the same diameter, and connecting the two semi-circle shaped ends are a channel having the width of the diameter of the semi-circles. The diameter of the semi-circles may be equal to the ranges described herein with reference to the circular shapedfluid passages 410. Referring toFIG. 2 , in such an embodiment, the portion of thecover plate 400 situated between adjacent circularly shapedfluid passages 410 could be eliminated, forming elongatedfluid passages 410. In embodiments, two, three, four, five, or even more circularly shaped fluid passages oriented in a line could be combined into anelongated fluid passage 410 by eliminating the portion of thecover plate 400 positioned therebetween. - In some embodiments, the
bottom support floor 500 may be substantially identical to thecover plate 400. In some of these embodiments, themagazine apparatus 100 may be stacked with anothermagazine apparatus 100 so that thebottom support floor 500 of atop magazine apparatus 100 serves as thecover plate 400 for abottom magazine apparatus 100. - Without being bound by theory, it is believed that
fluid passages 410 that are aligned with glassware-retainingopenings 210 allow for enhanced flow of fluids into and out of theglass articles 900, as compared with somecover plate 400 geometries with more open area for fluid flow. One measure of the ability of the vial to fill is the Bond number (Bo), which is a measure of the relative significance of buoyant forces compared with surface tension at the meniscus/fluid-air interface at the opening of the container. In order to drive filling of the vials with a processing fluid, such as molten salt, it may be desirable to have a large Bond number where buoyancy forces (bubble formation) dominate surface tension forces. In this case, the Bond number indicates a balance between surface tension and buoyant forces. The Bond number may be expressed as Bo=(ρgL2)/σ, where ρ=fluid density, g=acceleration due to gravity, L=characteristic length (radius of opening), and σ=surface tension of fluid. From this formula, in many embodiments, L is the most significant factor in whether a glass article fills, since the ratio of density to surface tension may be nearly constant for molten salt over the typical range of ion exchange temperatures. To this end it may be important to avoid any obstruction of the glass article mouth during filling. - One or more of the
bottom support floor 500, the glassware-securingmembers 200, thevertical supports 300, thecover plate 400 may be made of metal, such as stainless steel (e.g., 304L stainless steel). However, any material is suitable that can withstand the relatively high temperatures of the molten salt bath. In one embodiment, one or more components of themagazine apparatus 100 may be fabricated by laser or water jetting of raw stainless steel sheet material into the desired flat patterns and then forming and welding the sheets into their final shape. Thebottom support floor 500, the glassware-securingmembers 200, and/or thecover plate 400 may be electro-polished, which may deburr the sharp edges that may be created through the laser or water jetting process. Electro-polishing may also increase the surface finish which aids in the draining or sheeting of liquids from themagazine apparatus 100. In another embodiment, thebottom support floor 500, the glassware-securingmembers 200, and/or thecover plate 400 may be passivated following the electro-polishing, which may further increase the passive layer of the stainless steel to further increase the corrosion resistance of themagazine apparatus 100. - In another embodiment, two or
more magazine apparatuses 100 may be stacked adjacently and secured together in acassette 608 to form anassembly 110, as shown inFIG. 9 . In one embodiment, since two ormore magazine apparatuses 100 are in contact with one another, thebottom support floor 500 of a higher positionedmagazine apparatus 100 can serve as thecover plate 400 for amagazine apparatus 100 positioned below. In such an embodiment, only onecover plate 400 perassembly 110 may be included. In such an embodiment, thebottom support floor 500 may havefluid passages 510, such as those described in relation to thecover plate 400, and may be substantially identical to thecover plate 400 of theuppermost magazine apparatus 100. For example, thebottom support floor 500 may comprisefluid passages 510 which have a diameter less than da and greater than dm of aglass article 900. In another embodiment, thecover plate 400 may be integrated with thecassette 608, such that only thetop magazine apparatus 100 loaded into thecassette 608 includes a cover plate. - When vertical pressure is applied to the
glass article 900, more stress may be present in thecurved bottom edge 918 and acurved area 912 than theside wall 916 of the body. In embodiments, a surface scratch or other informality on thecurved bottom edge 918 and acurved area 912 may be more likely to propagate into a crack which may undesirably cause complete breakage of theglass article 900. In some embodiments, glassware-securingmembers 200 only contact theside wall 916 of theglass article 900, as shown inFIG. 9 . - It should be understood that a
cover plate 400, as used herein, may include a bottom support floor of an adjacent apparatus. Thecover plate 400 may not be permanently fastened to themagazine apparatus 100, such as to allow for removal of theglass articles 900. Thecover plate 400 may be fastened to themagazine apparatus 100 by any suitable mechanical means, such as by fasteners, screws, bolts, or a geometry of thecover plate 400 andmagazine apparatus 1000 designed to stably hold thecover plate 400 to themagazine apparatus 100. - Now referring collectively to
FIGS. 1, 2, 10, and 11 , theglass articles 900 can be strengthened by ion-exchange while being held in the receivingvolumes 220 ofmagazine apparatuses 100.FIG. 10 contains a process flow diagram 501 of a method for strengtheningglass articles 900 by ion-exchange andFIG. 11 schematically depicts the process described in the flow diagram. In afirst step 502,glass tube stock 1000 formed from an ion-exchangeable glass composition is initially shaped into glass articles 900 (specifically glass vials in the embodiment depicted) using conventional shaping and forming techniques. Instep 504, theglass articles 900 are loaded intomagazine apparatuses 100 using amechanical magazine loader 602. Themagazine loader 602 may be a mechanical gripping device, such as a caliper or the like, which is capable of grippingmultiple glass articles 900 at one time. Alternatively, the gripping device may utilize a vacuum system to grip theglass articles 900. Themagazine loader 602 may be coupled to a robotic arm or other, similar device capable of positioning themagazine loader 602 with respect to theglass articles 900 and themagazine apparatus 100. The magazine loader 603 positionsindividual glass articles 900 in the receivingvolumes 220. - In a
next step 506, themagazine apparatus 100 loaded withglass articles 900 is transferred with a mechanical conveyor, such as aconveyor belt 606, overhead crane or the like, to a cassette loading area. Thereafter, instep 508, a plurality of magazine apparatuses 100 (one depicted) are loaded into acassette 608. While only onemagazine apparatus 100 is depicted inFIG. 11 , it should be understood that thecassette 608 is constructed to hold a plurality ofmagazine apparatuses 100, such as depicted inFIG. 9 , such that a large number ofglass articles 900 can be processed simultaneously. Eachmagazine apparatus 100 is positioned in thecassette 608 utilizing acassette loader 610. Thecassette loader 610 may be a mechanical gripping device, such as a caliper or the like, which is capable of gripping one ormore magazine apparatuses 100 at a time. Alternatively, the gripping device may utilize a vacuum system to grip themagazine apparatuses 100. Thecassette loader 610 may be coupled to a robotic arm or other, similar device capable of positioning thecassette loader 610 with respect to thecassette 608 and themagazine apparatuses 100. - In a next step 511, the
cassette 608 containing themagazine apparatuses 100 andglass articles 900 is transferred to an ion-exchange station and loaded into an ion-exchange tank 614 to facilitate chemically strengthening theglass articles 900. Thecassette 608 is transferred to the ion-exchange station with acassette transfer device 612. Thecassette transfer device 612 may be a mechanical gripping device, such as a caliper or the like, which is capable of gripping thecassette 608. Alternatively, the gripping device may utilize a vacuum system to grip thecassette 608. Thecassette transfer device 612 and attachedcassette 608 may be automatically conveyed from the cassette loading area to the ion-exchange station with an overhead rail system, such as a gantry crane or the like. Alternatively, thecassette transfer device 612 and attachedcassette 608 may be conveyed from the cassette loading area to the ion-exchange station with a robotic arm. In yet another embodiment, thecassette transfer device 612 and attachedcassette 608 may be conveyed from the cassette loading area to the ion-exchange station with a conveyor and, thereafter, transferred from the conveyor to the ion-exchange tank 614 with a robotic arm or an overhead crane. - Once the
cassette transfer device 612 and attachedcassette 608 are at the ion-exchange station, thecassette 608 and theglass articles 900 contained therein may optionally be preheated prior to submerging thecassette 608 and theglass articles 900 in the ion-exchange tank 614. In some embodiments, thecassette 608 may be preheated to a temperature greater than room temperature and less than or equal to the temperature of the molten salt bath in the ion-exchange tank 614. For example, theglass articles 900 may be preheated to a temperature from about 300° C.-500° C. However, it should be understood that the preheating step is optional due to the relatively low thermal mass of themagazine apparatuses 100 described herein. - Without being bound by theory, thermal uniformity of the
magazine apparatus 100 andglass articles 900 prior to introduction into the ion-exchange tank may be important to maintaining temperature of the salt bath in the tank. For example, introduction of room temperature vials into hot salt may result in a solidification of salt around the opening of theglass article 900. Additionally, as the Bond number formula suggests, the filling performance also correlates with the ratio of fluid density to surface tension, both of which are temperature sensitive properties. This ratio decreases with temperature, which also may improve filling performance. - The ion-
exchange tank 614 contains a bath ofmolten salt 616, such as a molten alkali salt, such as KNO3, NaNO3 and/or combinations thereof. In one embodiment, the bath of molten salt is 100% molten KNO3 which is maintained at a temperature greater than or equal to about 350° C. and less than or equal to about 500° C. However, it should be understood that baths of molten alkali salt having various other compositions and/or temperatures may also be used to facilitate ion-exchange of the glass articles. In some embodiments, themolten salt 616 should be held at a temperature as high as is possible given process constraints. Without being bound by theory, it is believed that a higher salt bath temperature may reduce the ratio of salt density to viscosity. - In
step 512, theglass articles 900 are ion-exchange strengthened in the ion-exchange tank 614. Specifically, the glass articles are submerged in the molten salt and held there for a period of time sufficient to achieve the desired compressive stress and depth of layer in theglass articles 900. As theglass articles 900 are submerged, the glass articles initially have positive buoyancy as air escapes from the interior volume of the glass articles and is replaced with molten salt. As theglass articles 900 rise due to the positive buoyancy, the glass articles are vertically retained in position by thebottom support floor 500,cover plate 400, and glassware-securingmembers 200. - In one embodiment, the
glass articles 900 may be held in the ion-exchange tank 614 for a time period sufficient to achieve a depth of layer of up to about 100 μm with a compressive stress of at least about 300 MPa or even 350 MPa. The holding period may be less than 30 hours or even less than 20 hours. However it should be understood that the time period with which the glass articles are held in thetank 614 may vary depending on the composition of the glass container, the composition of the bath ofmolten salt 616, the temperature of the bath ofmolten salt 616, and the desired depth of layer and the desired compressive stress. - In one embodiment, the glass articles are dipped into the ion-
exchange tank 614 while being held at a non-normal angle relative to the major axis of the glass article and the surface of the fluid in the tank (shown as a dashed line inFIG. 12 ). The non-normal angle is shown asangle 165 inFIG. 12 . The orientation of the vial can also affect the reliability of the filling process. Without being bound by theory, it is believed that a vial that is introduced normal to the fluid surface is more likely to form bubbles. This is caused by balancing the bubble buoyancy to the hydrostatic pressure of the fluid. When theglass article 900 is titled, the forces are not aligned, allowing the bubble to escape and the fluid to enter theglass article 900 more reliably with less cavitation. The magazine apparatuses 100 and processes described herein may allow a fixed, non-normal angle to be imparted on theglass articles 900 with respect to the surface of the salt bath during introduction into the salt bath. Furthermore, in some embodiments,glass articles 900 may be moved by buoyancy forces, and these buoyancy forces may partially tip the glass article within the glassware-retainingopenings 210 to achieve non-normal angles of theglass articles 900 with respect to the surface of the salt bath during introduction into the salt bath. Such motion caused by buoyancy forces may improve filling efficiency. - Additionally, the speed at which the glass article is submerged can cause changes in the reliability of the filling process. Generally, slower dipping speeds may more reliably fill the
glass articles 900. However, it may be possible to utilize higher submersion speeds if theglass article 900 is submerged at a non-normal angle. Referring again toFIG. 12 , in some embodiments, the speed of submersion may be increased asangle 165 is decreased. In some embodiments, it may be desirable to submerge theglass article 900 whereangle 165 is about 45°, such as from about 40° to about 50° or from about 35° to about 55°. In another embodiment,angle 165 may be about 0°, such that the opening of the glass article is substantially perpendicular to the surface of the ion-exchange bath. For example,angle 165 may be from about −5° to about 5° or from about −10° to about 10°. - After the
glass articles 900 are ion-exchange strengthened, thecassette 608 andglass articles 900 are removed from the ion-exchange tank 614 using thecassette transfer device 612 in conjunction with a robotic arm or overhead crane. During removal from the ion-exchange tank 614, the various fluid passages of themagazine apparatus 100 allow the molten salt within the magazine apparatus to readily drain from eachmagazine apparatus 100. After thecassette 608 is removed from the ion-exchange tank 614, thecassette 608 and theglass articles 900 are suspended over the ion-exchange tank 614 and thecassette 608 is rotated about a horizontal axis such that any molten salt remaining in theglass articles 900 is emptied back into the ion-exchange tank 614. As thecassette 608 is rotated, theglass articles 900 are maintained in its position in the ware receiving volume 125 by the ware keepers 120. Thereafter, thecassette 608 is rotated back to its initial position and the glass articles are allowed to cool prior to being rinsed. - The
cassette 608 andglass articles 900 are then transferred to a rinse station with thecassette transfer device 612. This transfer may be performed with a robotic arm or overhead crane, as described above, or alternatively, with an automatic conveyor such as a conveyor belt or the like. In anext step 514, thecassette 608 andglass articles 900 are lowered into a rinsetank 618 containing a water bath 620 to remove any excess salt from the surfaces of theglass articles 900. Thecassette 608 andglass articles 900 may be lowered into the rinsetank 618 with a robotic arm, overhead crane or similar device which couples to thecassette transfer device 612. Similar to the salt bath submersion, the glass articles initially have a positive buoyancy upon being submerged in the rinsetank 618. As theglass articles 900 rise due to the positive buoyancy, the glass articles are vertically retained in position. Theglass articles 900 may be dipped at a non-normal angle relative to the surface of the salt bath, as discussed with regards to dipping into the salt bath. - The
cassette 608 andglass articles 900 are then withdrawn from the rinsetank 618, suspended over the rinsetank 618, and thecassette 608 is rotated about a horizontal axis such that any rinse water remaining in theglass articles 900 is emptied back into the rinsetank 618. As thecassette 608 is rotated, theglass articles 900 are maintained in their position in the receivingvolume 220. In some embodiments, the rinsing operation may be performed multiple times before thecassette 608 andglass articles 900 are moved to the next processing station. - In one particular embodiment, the
cassette 608 and theglass articles 900 are dipped in a water bath at least twice. For example, thecassette 608 may be dipped in a first water bath and, subsequently, a second, different water bath to ensure that all residual alkali salts are removed from the surface of the glass article. The water from the first water bath may be sent to waste water treatment or to an evaporator. - In a
next step 516, themagazine apparatuses 100 are removed from thecassette 608 with thecassette loader 610. Thereafter, instep 518, theglass articles 900 are unloaded from themagazine apparatuses 100 with themagazine loader 602 and transferred to a washing station. Instep 520, the glass articles are washed with a jet ofde-ionized water 624 emitted from anozzle 622. The jet ofde-ionized water 624 may be mixed with compressed air. - Optionally, in step 521 (not depicted in
FIG. 10 ), theglass articles 900 are transferred to an inspection station where the glass articles are inspected for flaws, debris, discoloration and the like. - While the magazine apparatuses have been shown and described herein being used in conjunction with glass containers, such as glass vials, it should be understood that the magazine apparatuses may be used to hold and retain various other types of glass articles including, without limitation, Vacutainers®, cartridges, syringes, ampoules, bottles, flasks, phials, tubes, beakers, vials or the like, including both round-form glass articles and non-round-form glass articles.
- It should now be understood that the magazine apparatuses and methods described herein may be used to hold and retain glass articles during processing. The magazine apparatuses restrict movement of the glass articles while allowing for ion-exchange processing by contact with molten salt baths.
- It will be apparent to those skilled in the art that various modifications and variations can be made to the embodiments described herein without departing from the spirit and scope of the claimed subject matter. Thus it is intended that the specification cover the modifications and variations of the various embodiments described herein provided such modification and variations come within the scope of the appended claims and their equivalents.
- The embodiments described herein will be further clarified by the following examples.
- Different patterns of cover plates were examined for their impact on vial filling, including a diagonal crisscrossing geometry, sometimes referred to herein as a “preform” geometry (as shown in
FIG. 6 ), a wire mesh geometry (as shown inFIG. 8 ), and a machined plate with holes specifically matched to each vial (the embodiment ofFIGS. 2 and 3 where the hole is larger than the glass article opening). Table 1 shows results of filling tests conducted with preform, wire mesh, and machined hole geometries. For each test, 162 glass vials were submerged and evaluated for whether they filled with fluid. -
TABLE 1 Test Number Cover Plate Geometry Fill % 1 Preform 90.1% 2 Wire Mesh 92.0% 3 Preform 71.0% 4 Wire Mesh 84.0% 5 Preform 68.5% 6 Wire Mesh 79.6% 7 Preform 56.8% 8 Wire Mesh 95.1% 9 Preform 96.8% 10 Machined holes 100.0% 11 Machined holes 99.3% 12 Machined holes 100.0% 13 Machined holes 100.0% 14 Machined holes 100.0% 15 Machined holes 100.0% 16 Machined holes 100.0% - The average fill rate for the preform geometry was 71.6%, 87.7% for the wire mesh geometry, and 99.9% for machined holes.
- Calculation were made to model glass vials dipped at varying immersion speeds and at varying angles into a fluid.
FIG. 13 depicts the calculated vial filling time at varying immersion speeds and angles of entry.Line 10 represents filling in 1 second,line 20 represents filling in 2 seconds,line 30 represents filling in 3 seconds, andline 40 represents filling in 4 seconds. The filling time is the time it took to completely fill the vial (without the presence of bubbles). The y-axis represents the immersion speed and the x-axis represents the vial angle, marked 165 inFIG. 12 . As reflected inFIG. 13 , higher immersion speeds require greater angles relative to the processing fluid surface. - It will be apparent to those skilled in the art that various modifications and variations can be made to the embodiments described herein without departing from the spirit and scope of the claimed subject matter. Thus it is intended that the specification cover the modifications and variations of the various embodiments described herein provided such modification and variations come within the scope of the appended claims and their equivalents.
Claims (20)
1. An apparatus for holding and retaining glass articles during processing, the apparatus defining a plurality of receiving volumes for holding glass articles and comprising:
a bottom support floor comprising a plurality of fluid passages;
a glassware-securing member positioned above the bottom support floor and comprising a plurality of glassware-retaining openings; and
a cover plate positioned above the glassware-securing member and comprising a plurality of fluid passages;
wherein:
each of the bottom support floor, the glassware-securing member, and the cover plate is substantially planar;
the bottom support floor, the glassware-securing member, and the cover plate are substantially parallel with one another;
each glassware-retaining opening of the glassware-securing member defines a width dimension of the receiving volume; and
the bottom support floor and the cover plate define a height dimension of the receiving volume.
2. The apparatus of claim 1 , further comprising vertical supports that securely connect the bottom support floor, the glassware-securing member, and the cover plate.
3. The apparatus of claim 1 , further comprising a second glassware-securing member positioned between the bottom support floor and the cover plate.
4. The apparatus of claim 1 , wherein the glassware-retaining openings of the glassware-securing member are circularly shaped.
5. The apparatus of claim 1 , wherein one or more of the fluid passages of the cover plate are aligned with a glassware-retaining opening.
6. The apparatus of claim 1 , wherein one or more of the fluid passages of the cover plate are circularly shaped.
7. The apparatus of claim 1 , wherein:
one or more of the fluid passages of the cover plate are aligned with a glassware-retaining opening;
one or more of the fluid passages of the cover plate are circularly shaped; and
a diameter of each fluid passage that is circularly shaped and aligned with a glassware-retaining opening is less than a diameter of glassware-retaining opening with which it is aligned.
8. The apparatus of claim 1 , wherein the cover plate and the bottom support floor are substantially identical.
9. An assembly for holding and retaining glass articles, the assembly comprising a plurality of magazine apparatuses, wherein one or more of the magazine apparatuses defines a plurality of receiving volumes and comprises:
a bottom support floor comprising a plurality of fluid passages;
a glassware-securing member positioned above the bottom support floor and comprising a plurality of glassware-retaining openings; and
a cover plate positioned above the glassware-securing member and comprising a plurality of fluid passages;
wherein:
each of the bottom support floor, the glassware-securing member, and the cover plate is substantially planar;
the bottom support floor, the glassware-securing member, and the cover plate are substantially parallel with one another;
each glassware-retaining opening of the glassware-securing member defines a width dimension of the receiving volume; and
the bottom support floor and cover plate define a height dimension of the receiving volume.
10. The assembly of claim 9 , wherein at least one of the magazine apparatuses do not comprise a cover plate.
11. The assembly of claim 9 , wherein for at least one magazine apparatus the height dimension of the receiving volume is defined by the bottom support floor of a lower magazine apparatus and a bottom support floor of an upper magazine apparatus, wherein the upper magazine apparatus and the lower magazine apparatus are stacked on one another and are adjacent to one another.
12. The assembly of claim 9 , where one or more of the magazine apparatuses further comprises vertical supports that securely connect the bottom support floor, the glassware-securing member, and the cover plate.
13. The assembly of claim 9 , where one or more of the magazine apparatuses further comprises a second glassware-securing member positioned between the bottom support floor and the cover plate.
14. The assembly of claim 9 , wherein the glassware-retaining openings of the glassware-securing member are circularly shaped.
15. The assembly of claim 9 , wherein one or more of the fluid passages of the cover plate are aligned with a glassware-retaining opening.
16. The assembly of claim 9 , wherein one or more of the fluid passages of the cover plate are circularly shaped.
17. The assembly of claim 9 , wherein:
one or more of the fluid passages of the cover plate are aligned with a glassware-retaining opening;
one or more of the fluid passages of the cover plate are circularly shaped; and
a diameter of each fluid passage that is circularly shaped and aligned with a glassware-retaining opening is less than a diameter of glassware-retaining opening with which it is aligned.
18. The assembly of claim 9 , wherein the cover plate and the bottom support floor are substantially identical.
19. A method for ion-exchanging glass articles comprising:
supplying an apparatus for holding and retaining glass articles during processing, the apparatus defining a plurality of receiving volumes for holding glass articles and comprising:
a bottom support floor comprising a plurality of fluid passages;
a glassware-securing member positioned above the bottom support floor and comprising a plurality of glassware-retaining openings; and
a cover plate positioned above the glassware-securing member and comprising a plurality of fluid passages;
wherein:
each of the bottom support floor, the glassware-securing member, and the cover plate is substantially planar;
the bottom support floor, the glassware-securing member, and the cover plate are substantially parallel with one another;
each glassware-retaining opening of the glassware-securing member defines a width dimension of the receiving volume; and
the bottom support floor and the cover plate define a height dimension of the receiving volume;
positioning one or more glass articles in one or more of the receiving volumes;
at least partially submerging the apparatus in an ion-exchange bath to contact the one or more glass articles with the ion-exchange bath.
20. The method of claim 19 , wherein the glass article is submerged in the ion-exchange bath at a non-normal angle relative to the surface of the ion-exchange bath.
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US20220002193A1 (en) * | 2020-07-06 | 2022-01-06 | Samsung Display Co., Ltd. | Strengthened Glass Manufacturing Apparatus and Strengthened Glass Manufacturing Method Using the Same |
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Also Published As
Publication number | Publication date |
---|---|
MX2017014309A (en) | 2018-03-01 |
TWI711592B (en) | 2020-12-01 |
WO2016183081A1 (en) | 2016-11-17 |
RU2017138382A (en) | 2019-06-11 |
TW201700422A (en) | 2017-01-01 |
CN107667079B (en) | 2020-07-31 |
US20180346377A1 (en) | 2018-12-06 |
CN107667079A (en) | 2018-02-06 |
JP6764419B2 (en) | 2020-09-30 |
EP3294681B1 (en) | 2021-08-25 |
US10669195B2 (en) | 2020-06-02 |
JP2018521938A (en) | 2018-08-09 |
EP3294681A1 (en) | 2018-03-21 |
RU2017138382A3 (en) | 2019-10-10 |
RU2716546C2 (en) | 2020-03-12 |
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