WO2010013692A1 - Composition à base de verre sans plomb - Google Patents

Composition à base de verre sans plomb Download PDF

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Publication number
WO2010013692A1
WO2010013692A1 PCT/JP2009/063388 JP2009063388W WO2010013692A1 WO 2010013692 A1 WO2010013692 A1 WO 2010013692A1 JP 2009063388 W JP2009063388 W JP 2009063388W WO 2010013692 A1 WO2010013692 A1 WO 2010013692A1
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WO
WIPO (PCT)
Prior art keywords
lead
glass
free glass
glass composition
component
Prior art date
Application number
PCT/JP2009/063388
Other languages
English (en)
Japanese (ja)
Inventor
卓也 高山
三紗子 桝井
寿文 山元
一郎 内山
Original Assignee
日本山村硝子株式会社
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 日本山村硝子株式会社 filed Critical 日本山村硝子株式会社
Priority to JP2010522717A priority Critical patent/JPWO2010013692A1/ja
Publication of WO2010013692A1 publication Critical patent/WO2010013692A1/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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
    • 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
    • C03C2207/00—Compositions specially applicable for the manufacture of vitreous enamels
    • C03C2207/08—Compositions specially applicable for the manufacture of vitreous enamels for light metals

Definitions

  • the present invention relates to a lead-free glass composition.
  • Glass and ceramics are usually used as an insulating material in electronic parts that require high reliability because they are less susceptible to thermal deterioration and have better electrical insulation than synthetic resins.
  • glass is used for coating metal members and bonding metal members. Moreover, it is used also for uses, such as sealing of the opening part of metal members.
  • glass in such applications is required to have a softening point and a thermal expansion coefficient according to the application, and to be excellent in chemical durability such as acid resistance and alkali resistance, and electrical insulation.
  • the thermal expansion coefficient it is required to show a high value in consideration of firing on a metal material such as copper, copper alloy, aluminum, and aluminum alloy.
  • Patent Document 1 describes a PbO-containing glass characterized by a thermal expansion coefficient in the range of 30 to 300 ° C. of 125 to 140 ⁇ 10 ⁇ 7 / ° C.
  • environmental problems have been pointed out in recent years for lead, and there is an increasing demand for lead-free glass compositions that do not substantially contain lead.
  • Patent Document 2 Bi 2 O 3 is used as a main component instead of PbO, and a large amount of an alkali metal oxide such as Li 2 O, Na 2 O, K 2 O or the like is contained therein.
  • a glass composition for a magnetic head is described.
  • the glass composition described here contains only alkali metal oxides such as Li 2 O, Na 2 O and K 2 O as components other than glass formers such as Bi 2 O 3 and SiO 2.
  • Patent Document 3 listed below describes a bismuth-based glass composition suitable for bonding, sealing, coating, and the like of electronic components.
  • this patent document 3 aims to provide a glass that does not have a risk of lowering electrical insulation. And the glass comprised from the composition specifically described in this patent document 3 has a low thermal expansion coefficient. Thus, a glass composition useful for forming a glass that does not contain lead and has a low softening point and has both excellent chemical durability and a high thermal expansion coefficient has not been found.
  • an object of the present invention is to provide a lead-free glass composition capable of forming a glass having a high thermal expansion coefficient and excellent chemical durability while having a low softening point.
  • the present inventors have found that a predetermined amount of a predetermined substance is contained as a glass component of the lead-free glass composition, and a high thermal expansion coefficient while having a low softening point. It has been found that a glass having excellent chemical durability can be formed, and the present invention has been completed. That is, according to the present invention, Bi 2 O 3 : 30 to 62%, SiO 2 : 10 to 35%, Al 2 O 3 : 0.1 to 5%, B 2 O 3 : 0.1 to 4.% by weight. 5% and TiO 2 : 0.1 to 8%, and a glass component containing a total of 10 to 25% of any one or more of Li 2 O, Na 2 O and K 2 O is included. A lead-free glass composition is provided.
  • the lead-free glass composition of the present invention can form a glass having a high thermal expansion coefficient and excellent chemical durability while having a low softening point.
  • the lead-free glass composition in this embodiment contains a glass component and an inorganic filler component.
  • the glass component is a component for forming a portion that is normally in a glass state when lead-free glass is formed with the lead-free glass composition of the present embodiment, and the inorganic filler component is contained in the lead-free glass. Usually, it is a component contained in a crystallized state. Therefore, in the lead-free glass in which the lead-free glass composition of the present embodiment is used, the inorganic filler component is usually observed in a state of being dispersed in the form of a matrix composed of the glass component.
  • the glass component contains Bi 2 O 3 , SiO 2 , Al 2 O 3 , B 2 O 3 , and TiO 2 as essential components. Further, Li 2 O, is contained in the glass component as also essential ingredient any one or more of Na 2 O and K 2 O.
  • ZnO, BaO, MgO, CaO, SrO, ZrO 2 , SeO 2 , CeO 2 , Fe 2 O 3 , MnO 2 , CuO, CoO, SnO 2 , Sb 2 O 3 , V 2 O 5 , NiO, Cr 2 O 3 , TeO 2 and the like can be contained as optional components. These optional components can be contained in the glass component as long as the effects of the present invention are not significantly impaired by the addition thereof.
  • Bi 2 O 3 is an effective component for making the lead-free glass composition of the present embodiment have a low softening point, and the content of the glass component in any one of the range of 30 to 62% by weight. It is taken.
  • the content of Bi 2 O 3 in the glass component is any one of the above ranges. For example, if the content is less than 30%, the softening point of the lead-free glass composition increases, and the metal member This is because there is a possibility that it may be necessary to perform baking at a temperature exceeding 580 ° C., for example, in the case where it is necessary to perform baking on the substrate. That is, if firing at such a temperature is necessary, it is difficult to use an aluminum member as the metal member, which places great restrictions on the method of use.
  • the content of Bi 2 O 3 in the glass component is 62% or less. If the content exceeds 62%, even if the softening point can be sufficiently reduced, for example, This is because it may be difficult to set the coefficient of thermal expansion of the glass formed by this glass component to a high value of, for example, 140 ⁇ 10 ⁇ 7 / ° C. or higher. That is, the content of Bi 2 O 3 in the glass component is 62% or less, for example, to prevent distortion from occurring during firing on a metal member.
  • the content of Bi 2 O 3 in the glass component is preferably in the range of 30 to 62%, and in the range of 42 to 60%. Is more preferable.
  • “thermal expansion coefficient” means an average value in the range of 50 to 250 ° C. unless otherwise specified.
  • the SiO 2 is an effective component for stabilizing the formation of the glass state, and the content of the SiO 2 in the glass component is any one of 10 to 35% by weight.
  • the content of SiO 2 in the glass component is any of the above ranges. For example, when the content is less than 10%, it is difficult to impart sufficient chemical durability to the lead-free glass composition. If it exceeds 35%, the firing temperature of the lead-free glass composition may exceed 580 ° C.
  • the content of SiO 2 in the glass component is preferably in the range of 15 to 30%, more preferably in the range of 16 to 25%. preferable.
  • the contents of Bi 2 O 3 and SiO 2 are preferably selected so that the total amount is in the range of 55 to 80% by weight. If the total amount is less than 55%, the glass becomes unstable and the chemical durability may be lowered. In this respect, the total amount of Bi 2 O 3 and SiO 2 is preferably in the range of 60 to 78%, and preferably in the range of 65 to 75%. Further preferred.
  • the Al 2 O 3 is an effective component for stabilizing the formation of the glass state and making the lead-free glass composition excellent in chemical durability, and the content in the glass component is 0% by weight. .1 to 5%.
  • the content of Al 2 O 3 in the glass component is any of the above ranges. For example, when the content is less than 0.1%, sufficient chemical durability is imparted to the lead-free glass composition. This is because it is difficult to do so, and if it exceeds 5%, the glass component may be destabilized, such as devitrification. Furthermore, when it exceeds 5%, the firing temperature of the lead-free glass composition may exceed 580 ° C.
  • the content of Al 2 O 3 in the glass component is preferably in the range of 0.1 to 5%. Furthermore, 0.1 to 3.0% is preferable.
  • the B 2 O 3 is an effective component for stabilizing the formation of the glass state and making the lead-free glass composition have a low softening point, and the content of the B 2 O 3 in the glass component is 0.1 to 4.% by weight.
  • One of the ranges of 5% is used.
  • the content of B 2 O 3 in the glass component is any of the above ranges because, for example, if the content is less than 0.1%, the stability in the glass state such as devitrification is reduced. This is because if the content exceeds 4.5%, it may be difficult to impart sufficient chemical durability to the lead-free glass composition.
  • the content of B 2 O 3 in the glass component is preferably in the range of 2.5 to 3.7%. Furthermore, 3.0 to 3.6% is preferable.
  • the TiO 2 is an effective component for making the lead-free glass composition excellent in chemical durability, and the content of the TiO 2 in the glass component is any one in the range of 0.1 to 8% by weight. It is taken.
  • the content of TiO 2 in the glass component is set to any of the above ranges, for example, when the content is less than 0.1%, sufficient chemical durability is imparted to the lead-free glass composition. This is because it is difficult to cause crystallization when the content exceeds 8%.
  • the content of TiO 2 in the glass component is preferably in the range of 1 to 8%, and is in the range of 1.1 to 8%. Is more preferable.
  • any one or more of Li 2 O, Na 2 O and K 2 O are effective components for lowering the softening point of the lead-free glass composition as described above, and in the lead-free glass composition, It is an effective component for imparting a high thermal expansion coefficient.
  • the total content of the glass components is usually in the range of 10 to 25% by weight percentage. In addition, these components should just contain any 1 type in them, and 2 types or all 3 types may contain them. The total content of these is considered to be any of the above ranges, for example, if the total content is less than 10%, the firing temperature of the lead-free glass composition may exceed 580 ° C., and exceeds 25%. This is because it may be difficult to impart sufficient chemical durability to the lead-free glass composition. In this respect, it is preferable that the total content of any one or more of Li 2 O, Na 2 O, and K 2 O is in the range of 15 to 20%.
  • ZnO is an effective component for making the lead-free glass composition have a low softening point, and even if it is contained in a glass component at a content of 10% or less by weight, There is little risk of significantly impairing the effects of the invention.
  • the content exceeds 10%, the glass component may be crystallized.
  • the content is preferably in the range of 2 to 6%.
  • BaO is an effective component for imparting a high thermal expansion coefficient to the lead-free glass composition, and is usually contained in the glass component at a content of 15% or less by weight.
  • the content is preferably 10% or less, more preferably 6% or less.
  • alkaline earth metal oxides other than BaO are effective components for stabilizing the formation of the glass state and effective for lowering the softening point of the lead-free glass composition.
  • the effect of the present invention is not significantly impaired.
  • the softening point of the lead-free glass composition may be increased, and firing at 580 ° C. or less may be difficult, and the glass component may become unstable in a glass state. There is also a risk that
  • ZrO 2 is an effective component for adjusting the viscosity and thermal expansion coefficient during softening of the lead-free glass composition, and is usually contained in the glass component in an amount of 5% or less by weight.
  • the content exceeds 5%, the glass component may be crystallized.
  • SeO 2 , CeO 2 , Fe 2 O 3 , MnO 2 , CuO, CoO, SnO 2 , Sb 2 O 3 , V 2 O 5 , NiO, Cr 2 O 3 , TeO 2 and the like are Even if the total content is contained in the glass component in an amount of 2% or less by weight percentage, the effect of the present invention is not significantly impaired.
  • the lead-free glass composition of the present invention is composed of each component.
  • the composition include a) Bi 2 O 3 : 42 to 60% by weight as composition X, and b) SiO 2 : 16 to 25% by weight, c) Al 2 O 3 : 0.1 to 5% by weight, d) B 2 O 3 : 3 to 3.6% by weight, e) TiO 2 : 1.1 to 8% by weight, f ) Na 2 O: 5.0 ⁇ 10% by weight, and g) K 2 O: 5.0 include compositions containing ⁇ 10 wt%.
  • composition A a) Bi 2 O 3 : 42 to 45% by weight, b) SiO 2 : 22 to 25% by weight, c) Al 2 O 3 : 0.1 to 1% by weight, d) B 2 O 3: 3 ⁇ 3.6 wt%, e) TiO 2: 5 ⁇ 8 wt%, f) Na 2 O: 7.0 ⁇ 10 wt%, g) K 2 O: 8.0 ⁇ 10 weight %) And h) a composition containing 4 to 6% by weight of BaO, or composition B: a) Bi 2 O 3 : 50 to 58% by weight, b) SiO 2 : 20 to 23% by weight, c) Al 2 O 3 D) B 2 O 3 : 3 to 3.6 wt%, e) TiO 2 : 5.1 to 8 wt%, f) Na 2 O: 5.0 to 10 wt% And g) K 2 O: A composition containing 5.0 to 10% by weight can be exemplified
  • composition X, composition A, and composition B are particularly preferable in terms of water resistance, acid resistance, and thermal expansion coefficient.
  • the lead-free glass composition of the present embodiment is substantially composed of only the substances specifically mentioned in the above-mentioned composition X, composition A, composition B and the like. It is preferable in that it can provide a high thermal expansion coefficient.
  • the lead-free glass composition in the present embodiment contains at least one of TiO 2 , Al 2 O 3 , SiO 2 , ZrO 2 , MgO, CaF, and BaF as the inorganic filler component.
  • These inorganic filler components are usually contained in the lead-free glass composition as a granular material, for example, TiO 2 particles, Al 2 O 3 particles, SiO 2 particles, ZrO 2 particles, MgO particles, CaF particles, and BaF.
  • the lead-free glass composition may contain inorganic particles such as particles.
  • the inorganic filler component can be contained in the form of inorganic particles, and the lead-free glass composition of the present embodiment is, for example, a mixture of glass particles (powder glass) composed of the glass components and the inorganic particles. Can be formed.
  • the inorganic filler component usually, inorganic particles having an average particle diameter (D 50 ) of 0.3 to 3.0 ⁇ m can be used.
  • D 50 average particle diameter
  • the ratio of the inorganic filler component to the total amount of this inorganic filler component and the said glass component is 20% or less by weight percentage.
  • the lead-free glass composition of the present embodiment is used for the formation of a glass film, and when an acidic or alkaline liquid is contacted with the surface, a part of the glass component is dissolved in the liquid and the surface side Even when eroded, the inorganic particles function to protect the inner side. That is, since the lead-free glass composition of the present embodiment contains such an inorganic filler component in addition to the glass component, chemical stability is further improved. Moreover, the said inorganic filler component can also be made to act as an extender, and is useful also for adjustment of the color tone of a lead-free glass composition.
  • the lead-free glass composition of the present embodiment has high chemical stability, the effect of the lead-free glass composition is more prominent when used to form the surface of a member subjected to a plating process, an etching process, or the like. Can do. Moreover, since it has a high thermal expansion coefficient, it can be suitably used not only for applications covering metal members, but also for applications such as adhesion between metal members and sealing of metal members. Moreover, since it has a low softening point, it can be fired at 580 ° C. or lower, and can be suitably used particularly in the above applications of aluminum and aluminum alloy members.
  • the lead-free glass composition in the present embodiment is excellent in chemical stability, it can be said that the lead-free glass composition is suitable for a covering material for these members.
  • the effect excellent also in the compounding use to conductor paste and resistor paste, such as Ag and Al, can be exhibited. Furthermore, it can be suitably used not only for metal members but also for sealing high-expansion ceramic members and for surface coating of high-expansion ceramic members. Moreover, it can be used suitably also for the adhesive use of the members made from high expansion ceramics, or the high expansion ceramics and metal members.
  • the lead-free glass composition of this embodiment can be made into various forms in addition to the powder state containing glass particles and inorganic particles. Further, in the present embodiment, the lead-free glass composition is described by exemplifying the case where the glass component and the inorganic filler component are included. However, the lead-free glass composition including only the glass component exemplified above is also the intent of the present invention. It is the range to do.
  • ⁇ Preparation of lead-free glass composition The blended raw materials were prepared so as to have the compositions shown in Tables 1 to 3, and after mixing, they were melted at a temperature of about 1000 to 1200 ° C. for 1 to 2 hours using a platinum crucible. The molten glass was quenched with a stainless steel cooling roll to produce glass flakes composed of a lead-free glass composition. The obtained glass flakes were further pulverized and classified by airflow, adjusted to become powdered glass having an average particle size (D 50 ) of 0.5 to 2.0 ⁇ m, and subjected to each evaluation. Further, based on the lead-free glass composition of Example 1 in Table 1 and Example 16 of Table 2, the lead-free glass compositions of Examples 9 to 13 and Examples 18 to 21 further containing an inorganic filler component were produced. did.
  • a powder sample using the lead-free glass composition of each example and comparative example was used as a sample for differential thermal analysis (DTA).
  • the powdery sample was press-molded and fired at (softening point + 50 ° C.) for 15 minutes, and then a rod-shaped sample having a diameter of 5 mm ⁇ length of 15 to 20 mm was prepared and used as a sample for measuring a thermal expansion coefficient. Further, the powder sample was fired to prepare a block sample having a height of 5 mm, a width of 10 mm, and a length of 15 mm, and used as a sample for evaluating chemical stability (water resistance, acid resistance).
  • the lead-free glass composition of the present invention can form a glass having a high thermal expansion coefficient and excellent chemical durability while having a low softening point.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

La présente invention concerne une composition à base de verre sans plomb qui vise à résoudre le problème de fournir une composition de verre sans plomb capable de former du verre qui, tout en ayant un point de ramollissement faible, présente également un coefficient élevé de dilatation thermique et une excellente durabilité chimique. La composition de verre sans plomb comporte 30-62% de Bi203, 10-35% de SiO2, 0,1-5% de Al203, 0,1-4,5% de B203, and 0,1-8% de TiO2 en poids ainsi qu’un constituant de verre contenant un total de 10 à 25% en poids d’un ou de plusieurs éléments parmi Li20, Na20, ou K20.
PCT/JP2009/063388 2008-07-28 2009-07-28 Composition à base de verre sans plomb WO2010013692A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2010522717A JPWO2010013692A1 (ja) 2008-07-28 2009-07-28 無鉛ガラス組成物

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008193689 2008-07-28
JP2008-193689 2008-07-28

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WO2010013692A1 true WO2010013692A1 (fr) 2010-02-04

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WO (1) WO2010013692A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011178574A (ja) * 2010-02-26 2011-09-15 Tokan Material Technology Co Ltd 低温焼成可能な高耐酸性コーティング用ガラス組成物、および同ガラス組成物ペースト
JP2011213526A (ja) * 2010-03-31 2011-10-27 Nihon Yamamura Glass Co Ltd ガラス組成物
JP2016119492A (ja) * 2011-03-07 2016-06-30 ショット アクチエンゲゼルシャフトＳｃｈｏｔｔ ＡＧ ハウジング

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06234547A (ja) * 1992-12-18 1994-08-23 Asahi Glass Co Ltd セラミックカラー組成物およびそれを使用する曲面ガラス板の製造法
JPH09227214A (ja) * 1996-02-22 1997-09-02 Asahi Glass Co Ltd セラミックカラー組成物
JPH09278483A (ja) * 1996-04-05 1997-10-28 Nippon Electric Glass Co Ltd ビスマス系ガラス組成物
JPH11343141A (ja) * 1998-04-27 1999-12-14 Cerdec Ag Keramische Farben 高ビスマス含量を有する、低溶融性で鉛不含のガラス―及びエナメル組成物

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06234547A (ja) * 1992-12-18 1994-08-23 Asahi Glass Co Ltd セラミックカラー組成物およびそれを使用する曲面ガラス板の製造法
JPH09227214A (ja) * 1996-02-22 1997-09-02 Asahi Glass Co Ltd セラミックカラー組成物
JPH09278483A (ja) * 1996-04-05 1997-10-28 Nippon Electric Glass Co Ltd ビスマス系ガラス組成物
JPH11343141A (ja) * 1998-04-27 1999-12-14 Cerdec Ag Keramische Farben 高ビスマス含量を有する、低溶融性で鉛不含のガラス―及びエナメル組成物

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011178574A (ja) * 2010-02-26 2011-09-15 Tokan Material Technology Co Ltd 低温焼成可能な高耐酸性コーティング用ガラス組成物、および同ガラス組成物ペースト
JP2011213526A (ja) * 2010-03-31 2011-10-27 Nihon Yamamura Glass Co Ltd ガラス組成物
JP2016119492A (ja) * 2011-03-07 2016-06-30 ショット アクチエンゲゼルシャフトＳｃｈｏｔｔ ＡＧ ハウジング
US9807897B2 (en) 2011-03-07 2017-10-31 Schott Ag Glass system for hermetically joining Cu components, and housing for electronic components

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