WO2007065874A1 - Procede de fabrication de verre plat par la methode de flottage ainsi que levre deversoir (spout lip) utilisee dans la methode de flottage - Google Patents

Procede de fabrication de verre plat par la methode de flottage ainsi que levre deversoir (spout lip) utilisee dans la methode de flottage Download PDF

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Publication number
WO2007065874A1
WO2007065874A1 PCT/EP2006/069258 EP2006069258W WO2007065874A1 WO 2007065874 A1 WO2007065874 A1 WO 2007065874A1 EP 2006069258 W EP2006069258 W EP 2006069258W WO 2007065874 A1 WO2007065874 A1 WO 2007065874A1
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WO
WIPO (PCT)
Prior art keywords
glass
lip
refractory material
weight
less
Prior art date
Application number
PCT/EP2006/069258
Other languages
German (de)
English (en)
Inventor
Jörg WITTE
Janusz Zborowski
Joachim Disam
Katharina LÜBBERS
Andreas Roters
Günter Fiederling
Original Assignee
Schott Ag
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 Schott Ag filed Critical Schott Ag
Priority to DE112006003321T priority Critical patent/DE112006003321B4/de
Publication of WO2007065874A1 publication Critical patent/WO2007065874A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • C03B5/26—Outlets, e.g. drains, siphons; Overflows, e.g. for supplying the float tank, tweels
    • C03B5/265—Overflows; Lips; Tweels
    • C03B5/267—Overflows; Lips; Tweels specially adapted for supplying the float tank
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/101—Refractories from grain sized mixtures
    • C04B35/106—Refractories from grain sized mixtures containing zirconium oxide or zircon (ZrSiO4)
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/486—Fine ceramics

Definitions

  • the invention relates to a method for producing
  • Liquid glass which is brought out of the work tub by means of a gutter, is allowed to flow onto a bath of molten metal, generally tin.
  • the flow rate of the glass is regulated by a movable slide (tweel), with which, among other things, the glass thickness is also adjusted. Seen behind the glass in the direction of flow
  • the spout lip is located on the slide, from which the glass melt flows continuously onto the metal melt, where it is formed into a dimensionally stable glass band and solidifies, the solidified glass band then being removed from the metal bath.
  • JP 33 85 539 describes a spout lip which consists of HZFC material (HZFC: High Zirconia Fused Cast) with a ZrO 2 content of 85-97% and the rest of a glassy material. These materials reduce the number of stripes and holes on the underside of the glass ribbon and the service life of the Spout Lip in the manufacture of high-melting glasses can be increased to around a year.
  • HZFC material High Zirconia Fused Cast
  • ZrO 2 content 85-97%
  • a disadvantage of the HZFC material is its low resistance to temperature changes, so that when the temperature changes, flaking in the surface can easily occur, in extreme cases even cracks, which lead to quality defects in the glass.
  • Another disadvantage is the high price for HZFC.
  • a ZrSiO 4 refractory material for the overflow fusion process is known from US 2005/0130830 A1, to which Fe 2 O 3 (in addition to the impurities already present) has been added in order to improve the deflection behavior.
  • this material shows a significantly increased interaction with the glass melt at high glass temperatures from approximately 1250 ° C.
  • DE 42 43 538 describes a zircon material which has good corrosion resistance to boric acid-containing glass melts at high temperatures. This material is made by adding phosphorus compounds and TiÜ 2 as sintering aids.
  • a spout lip which consists of a SiO 2 ceramic which is provided on its side which comes into contact with the glass flow with a metal layer made of molybdenum or tungsten.
  • a ceramic layer is also provided between the SiO 2 ceramic and the metal layer, which is intended to prevent the back attack by diffusing oxygen on the metal.
  • Magnesium aluminate spinel described which is coated on its top with a noble refractory metal, generally platinum or a platinum alloy.
  • a gas-tight diffusion barrier is also arranged between the metal and the spinel.
  • melt-cast lipstones often cause problems when they come from one
  • melt cast block are worked out or if they are to be ground to exact dimensions for high precision of the glass ribbon to be produced.
  • melt-cast AZS materials Al 2 O 3 -ZrO 2 -SiO 2
  • ZrO 2 melt-cast AZS materials with a proportion of 41% by weight ZrO 2 in the area of the mold bottom have a significantly higher proportion of zirconium oxide than in the head of the stone.
  • mold walls usually form a very fine-grained structure.
  • the solidification is delayed in the interior of the solidifying block, so that a coarse structure is usually formed there, which is partially interspersed with pores and in which the glass phase enriched with the impurities originating from raw materials is present in larger quantities, see Fig. 1 and Fig. 2
  • Figure 1 shows the fine structure of an HZFC material that forms near the mold wall in a melt-cast block
  • Figure 2 shows the much coarser structure inside the same block.
  • Polyvalent impurities such as TiO 2 and Fe 2 O 3 in particular can lead to blistering in glass contact. If the lip stone is carved out of a melt-cast block, it is
  • a reduction in the proportion of the glassy phase is only possible up to a certain limit, since the glassy phase is necessary for the casting and a refinement of the coarse structure through faster cooling new problems, e.g. Tension in the casting, entails. It is therefore necessary to pour the desired shape of the spout lip as precisely as possible in order to achieve a
  • the object of the invention is to find a process for the production of flat glass by the float process, with which very high quality qualities can be achieved even when using higher melting glasses, and a spout lip
  • a casting lip made of pressed and sintered refractory material from the group ZrO 2 , AI 2 O 3, ZrSiO 4 , with an Fe 2 O 3 content of less than
  • the refractory material is made of ZrO 2 or ZrSiO 4 and less than 0.2% by weight if the refractory material is made of Al 2 O 3 , because these materials have a very uniform structure with regard to grain size, glass phase and pore distribution.
  • ZrO 2 and ZrSiO 4 materials an Fe 2 O 3 content of at most 0.05% by weight is preferred, and in the case of Al 2 O 3 refractory materials of at most 0.1, in particular at most 0.08% by weight. %.
  • Fig. 1 Microstructure / structure of HZFC material, fine crystalline
  • Fig. 2 Microstructure / structure of HZFC material in the area of so-called "worm tracing": inhomogeneities in the structure enrichment of the glass phase;
  • Image 3 Microstructure / structure of pressed and sintered
  • Image 4 Microstructure / structure of pressed and sintered
  • Figure 5 Microstructure / structure of melt-cast aluminum alumina, relatively coarse crystalline structure
  • Figure 3 shows a polished section of a pressed and sintered ⁇ -aluminum oxide and Figure 4 shows a polished section of a pressed and sintered zirconium oxide.
  • the production of refractory ceramic products by pressing and sintering masses of appropriate composition is known per se and is also carried out in part on an industrial scale.
  • the casting lip according to the invention can also be produced by these well-known processes.
  • the pressing can be uniaxial, but isostatic pressing is preferred, with which better results are achieved with complicated shapes.
  • the hot isostatic pressing (HIP process) is also possible with good success, but is generally not popular due to the size of the casting lips to be pressed for economic reasons.
  • the material to be pressed should have such a grain size distribution that a very even structure is created during pressing.
  • the material to be pressed can, if necessary.
  • Known sintering aids such as SiO 2 , TiO 2 and stabilizers such as oxides from the group of lanthanides, in particular Y 2 O 3 or also CaO or MgO, can be added.
  • Stabilization is customary in particular in the case of a ZrO 2 ceramic and up to 10% by weight of Y 2 O 3 are added for full stabilization.
  • partially stabilized compositions with a correspondingly lower proportion of stabilizing oxides are also common.
  • the material After sintering, the material has an open porosity of up to 12%. An open porosity of up to 7%, in particular up to 2%, is preferred. Open porosities of around 0.5% can be achieved.
  • zirconium silicate materials for use as spout lip have a maximum density of 4.15 g ⁇ cm "3 with the corresponding porosity in order to ensure good resistance to temperature changes
  • the materials from which the spout lip is made should be as pure as possible. Impurities cannot always be completely excluded. TiO 2 or P 2 O 5 can generally be tolerated in each case up to about 1% by weight.
  • the P 2 O 5 content should preferably not exceed 0.4% by weight and the TiO 2 content should not exceed 0.8% by weight, in particular 0.5% by weight.
  • the total amount of the above-mentioned impurities should not exceed 1% by weight. Also prove to be isostatic
  • sintered materials containing zirconium oxide or zirconium silicate with a proportion of ZrO 2 of more than 60% and aluminum oxide with a proportion of Al 2 O 3 of at least 90% in glass contact are suitable.
  • zirconium as zirconium oxide or as zirconium silicate always contains a small proportion (usually 1.5-2.5% by weight) of hafnium oxide or silicate.
  • zirconium oxide content including the hafnium oxide content is therefore always understood.
  • a pressed and sintered aluminum oxide with a proportion of up to 20% by weight, in particular up to 10% by weight of zirconium oxide, can also be used.
  • materials with low electrical conductivity e.g. Zirconium silicate or ⁇ -alumina preferred as material for the spout lip.
  • pressed and sintered ceramics for example made of zirconium oxide or of aluminum oxide, can be used have lower blistering potential compared to melt-cast ⁇ / ⁇ -alumina, which is very often used as a spout lip material.
  • Figure 5 shows a section through a fused-cast ⁇ // - alumina is seen clearly the comparatively relatively coarse crystalline structure in which ⁇ next aR-Al 2 3 crystals also / -.? Al 2 O 3 crystals and small areas of Glass phase are recognizable. This material has a higher compared to pressed and sintered material
  • Blistering behavior between melt-cast alumina material and pressed and sintered ⁇ alumina material in contact with alkali-free glass at a temperature of 1380 0 C is shown in Figure 6.
  • Blister formation was determined by the method of Dunkl et al .: A Novel Method for the Determination of the Blistering Rate at the Refractory / Glass Interface; UNITECR '89: Proc. Unified Int Techn. Conf. on Refractories, Annaheim CA, 1-4 Nov. 1989, Westerville, 1989, 795-806.
  • Figure 7 shows the positive influence of a low F ⁇ 2 ⁇ 3 content on the blistering rate of zirconium silicate materials in contact with a glass melt at a temperature of 1400 0 C.
  • a particular advantage of the spout lip found is that it can be processed by grinding and / or polishing without impairing its good properties. It is therefore possible to make a spout lip from the full, i.e. work out a pressed and sintered block of material and it is also possible to bring a pressed and sintered spout lip to the desired size by milling, grinding and / or polishing or to produce a particularly smooth and flat surface.
  • the spout lip found is particularly suitable for the production of glass, which has particularly high requirements with regard to
  • Melting point has as soda-lime glass.
  • Such glasses are in particular borosilicate glasses, alkali-free glasses, aluminosilicate glasses, aluminolithium silicate glasses and precursor glasses for glass ceramics.
  • the Spout Lip is particularly suitable for the production of
  • Borosilicate glass with a composition of (in% by weight on an oxide basis): 55-65 SiO 2 , 12-20 Al 2 O 3 , maximum 5 B 2 O 3 , 0-5 BaO, 3-9 CaO, 1-5 MgO and 1-5 SrO; for the production of display glass with a composition of 55-70 SiO 2 , 12-20 Al 2 O 3 , 5-15 B 2 O 3 , 0-6 BaO, 0-12 CaO, 0-7 MgO, 0-10 SrO.

Abstract

L’invention concerne un procédé de fabrication par flottage d’un verre spécial, tel que le verre de borosilicate, le verre exempt d’alcalis, le verre d’aluminosilicate, le verre pour vitrocéramique, ledit verre étant éjecté par une lèvre déversoir, notamment éjecté de manière isostatique, et le matériau réfractaire fritté étant moulé sur le bain de flottage. En tant que matériau réfractaire, ZrO2, Al2O3, ZrSiO4 sont utilisés, la teneur en Fe2O3 étant inférieure à 0,08 % en poids dans le matériau réfractaire à base de ZrO2 et dans le matériau réfractaire à base de ZrSiO4 et étant d’au plus 0,2 % en poids dans le matériau réfractaire à base d’Al2O3. Le matériau réfractaire éjecté et fritté présente notamment une distribution de taille de particule régulière et une structure homogène.
PCT/EP2006/069258 2005-12-05 2006-12-04 Procede de fabrication de verre plat par la methode de flottage ainsi que levre deversoir (spout lip) utilisee dans la methode de flottage WO2007065874A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE112006003321T DE112006003321B4 (de) 2005-12-05 2006-12-04 Verfahren zur Herstellung von Flachglas nach dem Floatverfahren sowie Gießlippe (Spout Lip) für das Floatverfahren

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005059193 2005-12-05
DE102005059193.0 2005-12-05

Publications (1)

Publication Number Publication Date
WO2007065874A1 true WO2007065874A1 (fr) 2007-06-14

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PCT/EP2006/069258 WO2007065874A1 (fr) 2005-12-05 2006-12-04 Procede de fabrication de verre plat par la methode de flottage ainsi que levre deversoir (spout lip) utilisee dans la methode de flottage

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DE (1) DE112006003321B4 (fr)
WO (1) WO2007065874A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3286157A4 (fr) * 2015-04-24 2018-12-05 Corning Incorporated Réfractaires en zircone liés et procédés de fabrication associés
CN116368108A (zh) * 2020-11-02 2023-06-30 法商圣高拜欧洲实验及研究中心 烧结的矾土产品

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3434661B1 (fr) 2011-03-11 2021-04-28 Saint-Gobain Ceramics&Plastics, Inc. Objet réfractaire
RU2570213C2 (ru) 2011-03-30 2015-12-10 Сэнт-Гобэн Керамикс Энд Пластикс, Инк. Огнеупорное изделие и способ его формования и использования
CN103492327A (zh) 2011-04-13 2014-01-01 圣戈本陶瓷及塑料股份有限公司 包括β氧化铝的耐火物体及其制造和使用方法
US9249043B2 (en) 2012-01-11 2016-02-02 Saint-Gobain Ceramics & Plastics, Inc. Refractory object and process of forming a glass sheet using the refractory object
CN115806439A (zh) 2015-02-24 2023-03-17 圣戈本陶瓷及塑料股份有限公司 耐火制品和制备方法

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DE1596613A1 (de) * 1965-11-03 1971-02-25 Pilkington Brothers Ltd Zusammengesetzter Regelschieber aus feuerfestem Werkstoff fuer Einrichtungen der Glasindustrie
US5407873A (en) * 1992-12-22 1995-04-18 Dyko Industriekeramik Gmbh Zirconium silicate brick and method for its production
DE4091550C2 (de) * 1989-09-08 2002-01-10 Corhart Refractories Co Zirkon enthaltende feuerfeste Materialien mit verbesserter Wärmeschockfestigkeit
DE10308031A1 (de) * 2002-03-06 2003-11-27 Schott Glas Vorrichtung zum Zuführen von Glasschmelze über einen Überlaufstein (Spout lip) bei der Herstellung von Floatglas
US20050130830A1 (en) * 2003-12-16 2005-06-16 Ames Donald J. Creep resistant zircon refractory material used in a glass manufacturing system

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Publication number Priority date Publication date Assignee Title
DE1596613A1 (de) * 1965-11-03 1971-02-25 Pilkington Brothers Ltd Zusammengesetzter Regelschieber aus feuerfestem Werkstoff fuer Einrichtungen der Glasindustrie
DE4091550C2 (de) * 1989-09-08 2002-01-10 Corhart Refractories Co Zirkon enthaltende feuerfeste Materialien mit verbesserter Wärmeschockfestigkeit
US5407873A (en) * 1992-12-22 1995-04-18 Dyko Industriekeramik Gmbh Zirconium silicate brick and method for its production
DE10308031A1 (de) * 2002-03-06 2003-11-27 Schott Glas Vorrichtung zum Zuführen von Glasschmelze über einen Überlaufstein (Spout lip) bei der Herstellung von Floatglas
US20050130830A1 (en) * 2003-12-16 2005-06-16 Ames Donald J. Creep resistant zircon refractory material used in a glass manufacturing system

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Title
DUNKL M.: "Feuerfeste Werkstoffe im Kontakt mit der Glasschmelze", November 1998, VERLAG DER DEUTSCHEN GLASTECHNISCHEN GESELLSCHAFT, OFFENBACH/MAIN, XP002423793 *
DUNKL M.: "Praxisnahes Prüfen des Korrosionsverhaltens gegenüber Glasschmelzen", November 1998, VERLAG DER DEUTSCHEN GLASTECHNISCHEN GESELLSCHAFT, OFFENBACH/MAIN, XP002423795 *
GEBHARDT F.: "Werkstoffwissenschaftliche Grundlagen und anlagespezifische Anforderungen", November 1998, VERLAG DER DEUTSCHEN GLASTECHNISCHEN GESELLSCHAFT, OFFENBACH/MAIN, XP002423794 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3286157A4 (fr) * 2015-04-24 2018-12-05 Corning Incorporated Réfractaires en zircone liés et procédés de fabrication associés
CN116368108A (zh) * 2020-11-02 2023-06-30 法商圣高拜欧洲实验及研究中心 烧结的矾土产品

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DE112006003321A5 (de) 2008-10-16
DE112006003321B4 (de) 2010-01-14

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