WO2011105246A1 - Procédé de fabrication d'un verre cristallin du système lasi - Google Patents

Procédé de fabrication d'un verre cristallin du système lasi Download PDF

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Publication number
WO2011105246A1
WO2011105246A1 PCT/JP2011/053089 JP2011053089W WO2011105246A1 WO 2011105246 A1 WO2011105246 A1 WO 2011105246A1 JP 2011053089 W JP2011053089 W JP 2011053089W WO 2011105246 A1 WO2011105246 A1 WO 2011105246A1
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WO
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Prior art keywords
glass
las
halogen
rare earth
earth oxide
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PCT/JP2011/053089
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English (en)
Japanese (ja)
Inventor
泰 藤澤
慎護 中根
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日本電気硝子株式会社
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Application filed by 日本電気硝子株式会社 filed Critical 日本電気硝子株式会社
Priority to CN2011800107075A priority Critical patent/CN102781864A/zh
Publication of WO2011105246A1 publication Critical patent/WO2011105246A1/fr

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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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents

Definitions

  • the present invention relates to a method for producing a LAS (Li 2 O—Al 2 O 3 —SiO 2 ) -based crystalline glass having excellent foam quality.
  • LAS-based crystallized glass such as transparent crystallized glass having a ⁇ -quartz solid solution as a main crystal and opaque crystallized glass having a ⁇ -spodumene solid solution as a main crystal is known as a low expansion crystallized glass. Since these LAS-based crystallized glasses are excellent in heat resistance and thermal shock resistance, they are widely used for cooking appliance top plates, stove windows, fire prevention windows, and the like.
  • the LAS-based crystallized glass is manufactured by first preparing raw material LAS-based crystallized glass by preparing, melting and molding the raw materials, and subjecting the LAS-based crystallized glass to crystallization treatment.
  • the glass excellent in foam quality can be obtained by performing a clarification process with respect to molten glass at the time of glass melting or after glass melting.
  • the LAS crystalline glass has a problem that it is difficult to clarify because the viscosity of the glass melt is high.
  • As 2 O 3 and Sb 2 O 3 have been used as fining agents in order to promote glass fining (see, for example, Patent Documents 1 and 2).
  • As 2 O 3 and Sb 2 O 3 are substances with a large environmental load, and in recent years, the amount of use has been reduced as much as possible, or has not been used.
  • halogens such as Cl, SnO 2 , SO 3 and the like are used alone or in combination as a clarifying agent replacing As 2 O 3 or Sb 2 O 3 (see, for example, Patent Document 3).
  • halogen is effective as a refining agent because it has a high refining effect and hardly causes unwanted coloring.
  • JP-A-6-329439 JP 2001-48582 A Japanese Patent Laid-Open No. 11-228180
  • halogen When halogen is used as a fining agent, a halogen-based gas is released from the glass when the glass is melted to produce a fining effect.
  • halogen has been problematic in that it tends to remain in glass and does not sufficiently exert its potential fining ability.
  • an object of the present invention is to provide a method for obtaining LAS-based crystalline glass having excellent foam quality by enhancing the clarification ability of halogen during glass melting.
  • the inventors of the present invention have improved the halogen refining effect by using halogen as a refining agent and adding specific components in the LAS crystalline glass production method. Therefore, the present invention is proposed.
  • the present invention by melting a raw material batch, SiO 2 55 to 75%, Al 2 O 3 17 to 27%, Li 2 O 3 to 6%, MgO 0 to 2% by mass as a composition. Contains ZnO 0-2%, TiO 2 2-5.5%, ZrO 2 0-3%, rare earth oxide 0.03-1%, halogen 0.01-0.2%, substantially As 2
  • the present invention relates to a method for producing an LAS-based crystalline glass.
  • the present inventors have found that when halogen clarification is performed during melting of LAS-based crystalline glass, the amount of halogen remaining in the glass can be reduced by adding a rare earth oxide. That is, the rare earth oxide promotes the diffusion of the halogen in the glass into the remaining bubbles, and the bubble diameter is increased to facilitate the rising of the bubbles, thereby enhancing the fining effect. Therefore, even if the addition amount of the clarifier and the halogen to be used is reduced, a clarification effect equivalent to or higher than the conventional one can be expected.
  • the halogen remaining in the glass can be reduced, so that such an effect that corrosion of the metal thin film hardly occurs can be obtained.
  • LAS-based crystalline glass refers to glass that precipitates as a main crystal LAS-based crystals such as ⁇ -quartz solid solution and ⁇ -spodumene solid solution by crystallization treatment.
  • the LAS-based crystalline glass production method of the present invention is characterized in that the rare earth oxide is Nd 2 O 3 or Er 2 O 3 .
  • the present invention relates to a LAS-based crystalline glass produced by any one of the above-described production methods.
  • the present invention has a composition by mass% of SiO 2 55 to 75%, Al 2 O 3 17 to 27%, Li 2 O 3 to 6%, MgO 0 to 2%, ZnO 0 to 2%, TiO 2 2 to 5.5%, ZrO 2 0 to 3%, rare earth oxide 0.03 to 1%, halogen 0.01 to 0.2%, substantially As 2 O 3 and Sb 2 O
  • the present invention relates to a LAS crystalline glass characterized by not containing 3 .
  • the present invention relates to a LAS-based crystallized glass obtained by crystallizing the LAS-based crystallized glass described above.
  • the LAS-based crystallized glass of the present invention is characterized in that a ⁇ -quartz solid solution or a ⁇ -spodumene solid solution is precipitated as a main crystal.
  • the composition is, by mass%, SiO 2 55 to 75%, Al 2 O 3 17 to 27%, Li 2 O 3 to 6%, MgO 0 to 2%, ZnO 0 to 2%, TiO 2 2 to Contains 5.5%, ZrO 2 0-3%, rare earth oxide 0.03-1%, halogen 0.01-0.2%, substantially free of As 2 O 3 and Sb 2 O 3
  • the present invention relates to a method for producing LAS-based crystalline glass. The reason why the composition of the LAS-based crystalline glass is limited in this way in the present invention will be described below. Unless otherwise specified, “%” in the following description means “% by mass”.
  • SiO 2 forms a glass skeleton and is a component constituting an LAS crystal.
  • the SiO 2 content is preferably 55 to 75%, 58 to 70%, particularly preferably 60 to 68%.
  • the content of SiO 2 is less than 55%, the thermal expansion coefficient tends to increase, and it becomes difficult to obtain crystallized glass excellent in thermal shock resistance. In addition, chemical durability tends to decrease.
  • the content of SiO 2 exceeds 75%, the meltability of the glass deteriorates, the viscosity of the glass melt increases, and it tends to be difficult to clarify or form the glass.
  • Al 2 O 3 forms a glass skeleton and is a component constituting an LAS crystal.
  • the content of Al 2 O 3 is preferably 17 to 27%, 19 to 25%, particularly preferably 20 to 23%.
  • the content of Al 2 O 3 is less than 17%, the thermal expansion coefficient tends to increase, and it becomes difficult to obtain crystallized glass excellent in thermal shock resistance. In addition, chemical durability tends to decrease.
  • the content of Al 2 O 3 is more than 27%, the meltability of the glass deteriorates, the viscosity of the glass melt increases, and it tends to be difficult to clarify or form the glass. Further, the mullite crystals tend to precipitate and the glass tends to devitrify, and the glass is easily damaged.
  • Li 2 O is a component that constitutes an LAS-based crystal, and has a great influence on crystallinity, and is a component that lowers the viscosity of glass and improves glass meltability and formability.
  • the Li 2 O content is preferably 3 to 6%, 3.3 to 5.5%, particularly preferably 3.5 to 5%.
  • mullite crystals precipitate and the glass tends to devitrify.
  • LAS-based crystals are difficult to precipitate, and it becomes difficult to obtain crystallized glass excellent in thermal shock resistance.
  • the meltability of the glass deteriorates or the viscosity of the glass melt increases, making it difficult to clarify or molding the glass.
  • the content of Li 2 O exceeds 6%, the crystallinity becomes too strong, and the glass tends to be devitrified, and the glass is easily broken.
  • MgO is a component that dissolves in the LAS crystal.
  • the MgO content is preferably 0 to 2%, 0 to 1.5%, particularly preferably 0.1 to 1.2%. If the content of MgO exceeds 2%, the crystallinity becomes too strong and tends to devitrify, and the glass tends to break.
  • ZnO like MgO, is a component that dissolves in the LAS crystal.
  • the content of ZnO is preferably 0 to 2%, 0 to 1.5%, particularly preferably 0.1 to 1.2%. If the ZnO content is more than 2%, the crystallinity becomes too strong, and thus the glass tends to devitrify when molded while being cooled slowly. As a result, the glass tends to be broken, so that it becomes difficult to form by, for example, the float process.
  • TiO 2 is a nucleation component for precipitating crystals in the crystallization process.
  • the content of TiO 2 is preferably 2 to 5.5%, 2 to 5.2%, particularly 2 to 5%.
  • the content of TiO 2 is more than 5.5%, the glass tends to devitrify and easily break.
  • the content of TiO 2 is less than 2%, crystal nuclei are not sufficiently formed, and coarse crystals may be precipitated and damaged.
  • ZrO 2 is a nucleation component for precipitating crystals in the crystallization step, like TiO 2 .
  • the ZrO 2 content is preferably 0 to 3%, 0.1 to 2.5%, particularly preferably 0.5 to 2.3%.
  • the content of ZrO 2 is more than 3%, the glass tends to be devitrified when it is melted, making it difficult to mold the glass.
  • the production method of the present invention is characterized in that the raw material batch contains 0.03 to 1% rare earth oxide and 0.05 to 1% halogen.
  • the rare earth oxide lanthanoid oxides such as Nd 2 O 3 , Er 2 O 3 , Gd 2 O 3 , and CeO 2 can be used.
  • Nd 2 O 3 and Er 2 O 3 have a particularly high effect of promoting the halogen refining ability, and it becomes easy to obtain a LAS-based crystalline glass excellent in foam quality.
  • the rare earth oxide content in the raw material batch is preferably 0.03 to 1%, particularly 0.05 to 0.8%. If the rare earth oxide content is less than 0.03%, it is difficult to obtain the effect of reducing the residual halogen content in the glass, and as a result, it is difficult to obtain a sufficient refining effect.
  • the rare earth oxide content in the LAS crystalline glass obtained by the production method of the present invention is the same as described above.
  • halogen As the halogen, Cl, Br, I, and F are used alone or in combination. Among them, it is preferable to use Cl because of its high fining ability and easy handling.
  • the halogen raw material include alkali halides (for example, NaCl, KCl, LiCl, etc.).
  • the halogen content in the raw material batch is preferably 0.05 to 1%, particularly preferably 0.1 to 0.8%. If the halogen content in the raw material batch is less than 0.05%, the clarification effect tends to be insufficient. On the other hand, even if the halogen content is more than 1%, the fining effect is not increased, and the residual halogen content in the glass is increased, so that the above-described problem of corrosion of the metal thin film tends to occur.
  • the halogen content in the LAS crystalline glass obtained by the production method of the present invention is preferably 0.2% or less, particularly preferably 0.15% or less.
  • the halogen content in the LAS crystalline glass is more than 0.2%, the above-described problem of corrosion of the metal thin film tends to occur.
  • the lower limit is not particularly limited, but is practically 0.01% or more.
  • the halogen content refers to the content as a halogen atom.
  • substantially does not contain means a level that is not actively used as a raw material and is mixed as an impurity, and specifically means that the content is 0.1% or less. .
  • the SnO 2 and SO 3 which is other fining component may be added.
  • SnO 2 has an effect of increasing the coloring of Fe or the like contained in the glass raw material as an impurity, it is desirable to keep it at 0.2% or less.
  • SO 3 is a component that promotes clarification by diffusing into bubbles in the glass, like halogen.
  • SO 3 also has the action of generating bubbles by causing reboil, so the remaining amount in the glass can be kept at 200 ppm or less. desirable.
  • B 2 O 3 may be added to suppress the growth of coarse crystals when crystallizing glass.
  • the upper limit is preferably made 2% or less.
  • P 2 O 5 is a component that promotes phase separation of the glass and assists the formation of crystal nuclei, and can be added to the glass in an amount of 0.1% or more.
  • the upper limit is desirably 3% or less.
  • Na 2 O, K 2 O, CaO, SrO and BaO in order to reduce the viscosity of the glass and improve the meltability and formability, it is possible to add Na 2 O, K 2 O, CaO, SrO and BaO in a total amount of 0.1 to 5%. .
  • CaO, SrO, and BaO are components which devitrify the glass when the glass is melted, it is preferable that the total amount of these components is 2% or less.
  • a coloring agent such as NiO, CoO, Cr 2 O 3 , Fe 2 O 3 , V 2 O 5 can be added up to 2% in total.
  • a raw material batch prepared by mixing the above components is melted at a temperature of 1550 to 1850 ° C., and then molded and annealed to obtain a LAS crystalline glass.
  • Various molding methods such as a float method, a press method, and a roll-out method can be applied depending on the target shape.
  • a crystallized glass is produced from the crystalline glass thus produced as follows.
  • the formed LAS-based crystalline glass is heat-treated at 600 to 800 ° C. for 1 to 5 hours to form crystal nuclei, and further heat-treated at 800 to 1100 ° C. for 0.5 to 3 hours.
  • By precipitating, LAS-based crystallized glass can be obtained.
  • heat treatment is performed at 800 to 950 ° C. for 0.5 to 3 hours to precipitate ⁇ -quartz solid solution.
  • crystal nuclei are formed and then heat treated at 1000 to 1100 ° C. for 0.5 to 3 hours.
  • the crystallized glass of the present invention is formed by precipitating LAS-based crystals as main crystals, it has a low coefficient of thermal expansion of about ⁇ 10 to 30 ⁇ 10 ⁇ 7 / ° C. (measurement range: 30 to 750 ° C.) and is heat resistant. Excellent mechanical strength.
  • the LAS-based crystallized glass and LAS-based crystallized glass of the present invention have a composition of mass%, SiO 2 55 to 75%, Al 2 O 3 17 to 27%, Li 2 O 3 to 6%, MgO 0 to 2 %, ZnO 0-2%, TiO 2 2-5.5%, ZrO 2 0-3%, rare earth oxide 0.03-1%, halogen 0.01-0.2%, It is characterized by not containing As 2 O 3 and Sb 2 O 3 .
  • the reason for limiting the composition in this way is as described above. In addition to these components, the above components can be appropriately contained.
  • the crystallized glass of the present invention may be subjected to post-processing such as cutting, polishing, bending, or painting on the surface.
  • raw material powders were prepared so as to have the composition shown in Table 1, and Nd 2 O 3 or Er 2 O 3 and Cl were added at the ratios shown in Tables 2 to 4 to obtain raw material batches.
  • Cl raw material NaCl was used in batches A and C, and LiCl was used in batch B.
  • Each raw material batch was put into a crucible and melted at 1600 ° C. for 20 hours and further at 1700 ° C. for 4 hours.
  • the glass melt was poured onto a carbon plate, leveled to a thickness of about 5 mm with a roller, and annealed with an electric furnace to obtain a glass sample.
  • the annealing was performed by lowering the temperature from 700 ° C. to room temperature at a rate of 100 ° C./hour.
  • Cl residual amount and clarity were evaluated. The results are shown in Tables 2-4.
  • components other than Cl had the contents shown in Tables 1 to 4.
  • the residual amount of Cl was measured by processing each glass sample into a 3 mm plate shape, mirror-polishing both surfaces, performing total elemental analysis by fluorescent X-ray analysis (XRF), and correcting for ZAF.
  • XRF fluorescent X-ray analysis
  • Clarity is “A” when the number of bubbles per 100 g (bubble diameter of 0.1 mm or more) of the glass sample is “A”, “B” when 1-2, and “5” when 3-5. “C”, 6 or more were evaluated as “D”.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)
  • Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)

Abstract

>L'invention concerne un procédé de fabrication d'un verre cristallin du système LAS par fusion d'un lot de matière première, le verre cristallin du système LAS comprenant, en % en masse, 55 à 75 % de SiO2, 17 à 27 % d'Al2O3, 3 à 6 % de Li2O, 0 à 2 % de MgO, 0 à 2 % de ZnO, 2 à 5,5 % de TiO2, 0 à 3 % de ZrO2, 0,03 à 1 % d'un oxyde des terres rares, et 0,01 à 0,2 % d'un atome d'halogène et ne contient sensiblement pas d'As2O3 ou Sb2O3, et le procédé étant caractérisé en ce que le lot de matière première contient 0,03 à 1 % de l'oxyde des terres rares et 0,05 à 1 % de l'halogène.
PCT/JP2011/053089 2010-02-24 2011-02-15 Procédé de fabrication d'un verre cristallin du système lasi WO2011105246A1 (fr)

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CN2011800107075A CN102781864A (zh) 2010-02-24 2011-02-15 Las系结晶玻璃的制造方法

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JP2010038224A JP2011173748A (ja) 2010-02-24 2010-02-24 Ｌａｓ系結晶性ガラスの製造方法
JP2010-038224 2010-02-24

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9359244B2 (en) 2013-05-21 2016-06-07 Colorado School Of Mines Alumina-rich glasses and methods for making the same
WO2023092260A1 (fr) * 2021-11-23 2023-06-01 海南大学 Verre microcristallin las basé sur la cristallisation directionnelle et procédé de préparation associé

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JP2013087986A (ja) * 2011-10-14 2013-05-13 Nippon Electric Glass Co Ltd 調理器用トッププレート用ガラス板及びその製造方法
DE102012202697A1 (de) * 2012-02-22 2013-08-22 Schott Ag Transparente farbarme Lithiumaluminiumsilikat-Glaskeramik und deren Verwendung
FR3002532B1 (fr) * 2013-02-28 2015-02-27 Eurokera Vitroceramique du type aluminosilicate de lithium contenant une solution solide de beta-spodumene
JP2015110508A (ja) 2013-10-31 2015-06-18 株式会社オハラ 結晶化ガラス
CN109015419B (zh) * 2018-08-02 2021-05-07 大连工业大学 一种las系微晶玻璃磨料结合剂配方、其制备方法及应用
CN113003939A (zh) * 2019-12-19 2021-06-22 湖州大享玻璃制品有限公司 SiO2-CaO系结晶化玻璃及其制造方法
JP7484369B2 (ja) * 2020-04-17 2024-05-16 Ａｇｃ株式会社 アルミノシリケートガラス及びその製造方法
JP7052956B1 (ja) 2020-10-19 2022-04-12 湖州大享玻璃制品有限公司 Ｌｉ２Ｏ－Ａｌ２Ｏ３－ＳｉＯ２系結晶化ガラス及びＬｉ２Ｏ－Ａｌ２Ｏ３－ＳｉＯ２系結晶性ガラス
CN115959830A (zh) * 2021-10-08 2023-04-14 湖州大享玻璃制品有限公司 一种SiO2-CaO系结晶化玻璃及其制造方法

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JP2007254277A (ja) * 2006-03-20 2007-10-04 Schott Ag 光学検出可能な、フロート可能な、ヒ素およびアンチモンを含まないグレイザブルなリチウム−アルミノケイ酸ガラス

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JP2006206430A (ja) * 2005-01-24 2006-08-10 Schott Ag ガラスまたはガラスセラミクスの施釉、ほうろう処理および加飾用の鉛フリーおよびカドミウムフリーガラス
JP2007254277A (ja) * 2006-03-20 2007-10-04 Schott Ag 光学検出可能な、フロート可能な、ヒ素およびアンチモンを含まないグレイザブルなリチウム−アルミノケイ酸ガラス

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9359244B2 (en) 2013-05-21 2016-06-07 Colorado School Of Mines Alumina-rich glasses and methods for making the same
WO2023092260A1 (fr) * 2021-11-23 2023-06-01 海南大学 Verre microcristallin las basé sur la cristallisation directionnelle et procédé de préparation associé

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JP2011173748A (ja) 2011-09-08

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