JP2001139344A - Leadless low melting point glass and glass frit - Google Patents

Leadless low melting point glass and glass frit

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Publication number
JP2001139344A
JP2001139344A JP31562299A JP31562299A JP2001139344A JP 2001139344 A JP2001139344 A JP 2001139344A JP 31562299 A JP31562299 A JP 31562299A JP 31562299 A JP31562299 A JP 31562299A JP 2001139344 A JP2001139344 A JP 2001139344A
Authority
JP
Japan
Prior art keywords
glass
less
melting point
low melting
sno
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.)
Granted
Application number
JP31562299A
Other languages
Japanese (ja)
Other versions
JP2001139344A5 (en
JP4061792B2 (en
Inventor
Yasuko Douya
康子 堂谷
Hiroshi Usui
寛 臼井
Tsuneo Manabe
恒夫 真鍋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AGC Inc
Original Assignee
Asahi Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to JP31562299A priority Critical patent/JP4061792B2/en
Publication of JP2001139344A publication Critical patent/JP2001139344A/en
Publication of JP2001139344A5 publication Critical patent/JP2001139344A5/ja
Application granted granted Critical
Publication of JP4061792B2 publication Critical patent/JP4061792B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
    • 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
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/19—Silica-free oxide glass compositions containing phosphorus containing boron

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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)
  • Inorganic Insulating Materials (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain leadless low melting point glass which is usable for adhesive sealing, coating, etc. of plasma display panels, fluorescent display tubes, etc. and of which the fired matter has an excellent electrical insulation characteristic. SOLUTION: This leadless low melting point glass consists of, by molar %, 15 to 50 P2O5, 2 to 35 SnO, 5 to 45 ZnO, 0.1 to 30 B2O3, <1 SnO/ZnO, 0 to 35 MgO+CaO+SrO+BaO, 0 to 10 Al2O3+In2O3+WO3 and 0 to 3 Li2O+Na2O +K2O.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、プラズマディスプ
レイパネル（ＰＤＰ）、蛍光表示管（ＶＦＤ）等のフラ
ットディスプレイパネルにおける封着、被覆、隔壁形成
に好適な無鉛低融点ガラスおよびガラスフリットに関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a lead-free low-melting glass and a glass frit suitable for sealing, coating, and forming barrier ribs in flat display panels such as plasma display panels (PDPs) and fluorescent display tubes (VFDs).

【０００２】[0002]

【従来の技術】ＰＤＰ、ＶＦＤの封着用、被覆用、また
は隔壁形成用のガラスフリットに用いられるガラス粉末
のガラスとして、電気絶縁性を低下させるおそれのある
アルカリ金属酸化物を含有することなく、または含有し
たとしても低含有量で、低軟化点を実現できるリン酸ス
ズ亜鉛系ガラスが注目されている。2. Description of the Related Art As glass of glass powder used for sealing, coating, or forming a partition wall of PDPs and VFDs, it does not contain an alkali metal oxide which may lower electric insulation. In addition, tin-zinc phosphate-based glass that can realize a low softening point with a low content even if it is contained has been attracting attention.

【０００３】[0003]

【発明が解決しようとする課題】従来知られているリン
酸スズ亜鉛系ガラスは焼成時に結晶化しやすく、２回以
上焼成・流動させて使う場合、２回目以降の焼成におい
て流動しにくい、または繰り返し焼成によって寸法安定
性が低下する、等の問題があった。本発明は、以上の課
題を解決し、２回以上焼成を行う用途にも適用できる無
鉛低融点ガラスおよびガラスフリットの提供を目的とす
る。The conventionally known tin-zinc phosphate glass is easily crystallized at the time of firing, and when used after firing and flowing more than once, it is difficult to flow at the second and subsequent firings, or repeated. There was a problem that dimensional stability was reduced by firing. An object of the present invention is to solve the above problems and to provide a lead-free low-melting glass and a glass frit that can be applied to applications where firing is performed twice or more.

【０００４】[0004]

【課題を解決するための手段】本発明は、下記酸化物基
準のモル％表示で、Ｐ2Ｏ5：１５〜５０、ＳｎＯ：２〜
３５、ＺｎＯ：５〜４５、Ｂ2Ｏ3：０．１〜３０、Ｍｇ
Ｏ：０〜３５、ＣａＯ：０〜３５、ＳｒＯ：０〜３５、
ＢａＯ：０〜３５、Ａｌ2Ｏ3：０〜１０、Ｉｎ 2Ｏ3：０
〜１０、ＷＯ3：０〜１０、Ｌｉ2Ｏ：０〜３、Ｎａ
2Ｏ：０〜３、Ｋ2Ｏ：０〜３、から実質的になり、Ｍｇ
Ｏ＋ＣａＯ＋ＳｒＯ＋ＢａＯが０〜３５モル％であり、
Ａｌ2Ｏ3＋Ｉｎ2Ｏ3＋ＷＯ3が０〜１０モル％であり、
Ｌｉ2Ｏ＋Ｎａ 2Ｏ＋Ｋ2Ｏが０〜３モル％であり、か
つ、ＳｎＯのＺｎＯに対するモル比が１未満である無鉛
低融点ガラス、および、低膨張セラミックスフィラーお
よび耐熱顔料の少なくともいずれか一方と、前記無鉛低
融点ガラスの粉末を含有するガラスフリットを提供す
る。According to the present invention, there is provided the following oxide group:
In terms of semi-mol%, PTwoOFive: 15-50, SnO: 2
35, ZnO: 5-45, BTwoOThree: 0.1 to 30, Mg
O: 0 to 35, CaO: 0 to 35, SrO: 0 to 35,
BaO: 0-35, AlTwoOThree: 0 to 10, In TwoOThree: 0
-10, WOThree: 0 to 10, LiTwoO: 0-3, Na
TwoO: 0-3, KTwoO: substantially consisting of 0 to 3, Mg
O + CaO + SrO + BaO is 0 to 35 mol%,
AlTwoOThree+ InTwoOThree+ WOThreeIs 0 to 10 mol%,
LiTwoO + Na TwoO + KTwoO is 0 to 3 mol%,
Lead-free, the molar ratio of SnO to ZnO is less than 1
Low melting glass and low expansion ceramic filler and
And at least one of the heat-resistant pigments and the lead-free low
Provide glass frit containing melting glass powder
You.

【０００５】[0005]

【発明の実施の形態】本発明の無鉛低融点ガラス（以下
単に本発明のガラスという。）を、封着、被覆、または
隔壁形成に用いるときは、粉末化して使用される。この
粉末化されたガラスは通常、必要に応じて低膨張セラミ
ックスフィラー、耐熱顔料、等と混合され、次にビヒク
ルと混練してペースト化される。このガラスペーストは
下地のガラスの所定部位に塗布され、焼成される。ここ
でいう下地のガラスは、ガラスの上に透明電導膜等が被
覆されているものも含む。BEST MODE FOR CARRYING OUT THE INVENTION When the lead-free low-melting glass of the present invention (hereinafter simply referred to as the glass of the present invention) is used for sealing, coating, or forming partition walls, it is used in the form of powder. This powdered glass is usually mixed with a low-expansion ceramic filler, a heat-resistant pigment, or the like, if necessary, and then kneaded with a vehicle to form a paste. This glass paste is applied to a predetermined portion of the underlying glass and fired. The base glass referred to here includes those in which a transparent conductive film or the like is coated on the glass.

【０００６】本発明のガラスの軟化点（Ｔs）は５８０
℃以下であることが好ましい。５８０℃超では、ＰＤ
Ｐ、ＶＦＤ、等の封着、被覆、または隔壁形成に用いる
ことが困難になるおそれがある。より好ましくは５６０
℃以下、特に好ましくは５５０℃以下である。また、Ｔ
sは５００℃以上であることが好ましい。５００℃未満
では、ＰＤＰ、ＶＦＤ、等における被覆または隔壁形成
に用いることが困難になるおそれがある。より好ましく
は５１０℃以上、特に好ましくは５２０℃以上、最も好
ましくは５３０℃以上である。The softening point (T s ) of the glass of the present invention is 580
It is preferable that the temperature is not higher than ° C. If the temperature exceeds 580 ° C, PD
It may be difficult to use P, VFD, or the like for sealing, coating, or forming a partition. More preferably 560
° C or lower, particularly preferably 550 ° C or lower. Also, T
s is preferably 500 ° C. or higher. If the temperature is lower than 500 ° C., it may be difficult to use it for coating or forming a partition in PDP, VFD, and the like. It is more preferably at least 510 ° C, particularly preferably at least 520 ° C, most preferably at least 530 ° C.

【０００７】本発明のガラスの結晶化温度（Ｔc）はＴs
よりも４０℃以上高いことが好ましい。ＴcとＴsの差
（Ｔc−Ｔs）が４０℃未満では焼成時に結晶化しやすく
なるおそれがある。ここで、Ｔcは示差熱分析（ＤＴ
Ａ）によって得られる結晶化ピーク温度であり、結晶化
ピークが認められない場合は、Ｔc＝∞とする。（Ｔc−
Ｔ s）は６０℃以上であることがより好ましく、７０℃
以上であることが特に好ましく、８０℃以上であること
が最も好ましい。The crystallization temperature (T) of the glass of the present inventionc) Is Ts
It is preferable that the temperature is higher by 40 ° C. or more than that. TcAnd TsDifference
(Tc-Ts) Is less than 40 ° C, it tends to crystallize during firing.
Could be. Where TcIndicates differential thermal analysis (DT
A) is the crystallization peak temperature obtained by A)
If no peak is observed, Tc= ∞. (Tc−
T s) Is more preferably 60 ° C. or more,
It is particularly preferable that the temperature is 80 ° C or higher.
Is most preferred.

【０００８】本発明のガラスの５０〜２５０℃における
線膨張係数は１２０×１０-7／℃以下であることが好ま
しい。１２０×１０-7／℃超では、後述の本発明のガラ
スフリットの焼成物の前記線膨張係数が大きくなりすぎ
るおそれがある。より好ましくは１１０×１０-7／℃以
下、特に好ましくは１００×１０-7／℃以下である。ま
た、前記線膨張係数は６０×１０-7／℃以上であること
が好ましい。以下、５０〜２５０℃における線膨張係数
を単に膨張係数という。The linear expansion coefficient of the glass of the present invention at 50 to 250 ° C. is preferably 120 × 10 −7 / ° C. or less. If it exceeds 120 × 10 −7 / ° C., the coefficient of linear expansion of a fired product of the glass frit of the present invention described below may be too large. It is more preferably at most 110 × 10 −7 / ° C., particularly preferably at most 100 × 10 −7 / ° C. Further, the coefficient of linear expansion is preferably 60 × 10 −7 / ° C. or more. Hereinafter, the coefficient of linear expansion at 50 to 250 ° C. is simply referred to as an expansion coefficient.

【０００９】次に、本発明のガラスの組成について、モ
ル％を単に％と記して以下に説明する。Ｐ2Ｏ5はネット
ワークフォーマであり、必須である。１５％未満ではガ
ラス化が困難になる。好ましくは２５％以上、より好ま
しくは２７％以上、特に好ましくは２８％以上である。
５０％超では化学的耐久性が低下する。好ましくは４０
％以下、より好ましくは３７％以下である。Next, the composition of the glass of the present invention will be described below by simply writing mol% as%. P 2 O 5 is a network former and is essential. If it is less than 15%, vitrification becomes difficult. It is preferably at least 25%, more preferably at least 27%, particularly preferably at least 28%.
If it exceeds 50%, the chemical durability decreases. Preferably 40
% Or less, more preferably 37% or less.

【００１０】ＳｎＯは軟化点を下げ流動性を増加させる
成分であり、必須である。２％未満では軟化点が高くな
りすぎる。好ましくは３％以上、より好ましくは７％以
上、特に好ましくは１５％以上である。３５％超ではガ
ラスの溶解性が低下し、溶融ガラス表面に被膜状の異物
層が形成される。好ましくは３０％以下、より好ましく
は２５％以下である。[0010] SnO is a component that lowers the softening point and increases the fluidity, and is essential. If it is less than 2%, the softening point becomes too high. It is preferably at least 3%, more preferably at least 7%, particularly preferably at least 15%. If it exceeds 35%, the solubility of the glass decreases, and a film-like foreign substance layer is formed on the surface of the molten glass. It is preferably at most 30%, more preferably at most 25%.

【００１１】ＺｎＯは、ガラスを安定化させる効果、化
学的耐久性を向上させる効果、膨張係数を低下させる効
果、または、軟化点を下げる効果を有し、必須である。
５％未満では前記効果が小さい。好ましくは２０％以
上、より好ましくは２４％以上、特に好ましくは２５％
以上である。４５％超では焼成時に結晶化しやすくな
る。好ましくは３５％以下、より好ましくは３２％未満
である。[0011] ZnO is essential because it has the effect of stabilizing the glass, the effect of improving the chemical durability, the effect of reducing the expansion coefficient, and the effect of lowering the softening point.
If it is less than 5%, the effect is small. Preferably at least 20%, more preferably at least 24%, particularly preferably at least 25%
That is all. If it exceeds 45%, it tends to crystallize during firing. Preferably it is 35% or less, more preferably less than 32%.

【００１２】ＳｎＯのＺｎＯに対するモル比、すなわち
ＳｎＯの含有量をＺｎＯの含有量で除した値は１未満で
なければならない。このモル比が１以上では、ガラスの
溶解性が低下し、溶融ガラス表面に被膜状の異物層が形
成される。好ましくは０．９７以下、より好ましくは
０．９３以下、特に好ましくは０．９０以下である。The molar ratio of SnO to ZnO, ie, the value obtained by dividing the SnO content by the ZnO content, must be less than 1. When the molar ratio is 1 or more, the solubility of the glass decreases, and a film-like foreign material layer is formed on the surface of the molten glass. Preferably it is 0.97 or less, more preferably 0.93 or less, particularly preferably 0.90 or less.

【００１３】Ｂ2Ｏ3はガラスを安定化し、また流動性を
増加させる効果を有し、必須である。０．１％未満では
前記効果が小さくなりすぎる。好ましくは０．５％以
上、より好ましくは１％以上である。３０％超では化学
的耐久性が低下する、またはガラスが不安定になる。好
ましくは２０％以下、より好ましくは１５％以下、特に
好ましくは１０％以下、最も好ましくは５％以下であ
る。B 2 O 3 has the effect of stabilizing the glass and increasing the flowability, and is essential. If it is less than 0.1%, the above effect is too small. Preferably it is 0.5% or more, more preferably 1% or more. If it exceeds 30%, the chemical durability is reduced or the glass becomes unstable. It is preferably at most 20%, more preferably at most 15%, particularly preferably at most 10%, most preferably at most 5%.

【００１４】ＭｇＯ、ＣａＯ、ＳｒＯおよびＢａＯはい
ずれも必須ではないが、ガラスを安定化するために、ま
たは焼成時の結晶化を抑制するために、それぞれ３５％
まで含有してもよい。３５％超では軟化点が高くなりす
ぎるおそれがある。より好ましくは１９％以下、特に好
ましくは１５％以下である。Although MgO, CaO, SrO and BaO are not essential, they are each 35% in order to stabilize the glass or to suppress crystallization during firing.
May be contained. If it exceeds 35%, the softening point may be too high. It is more preferably at most 19%, particularly preferably at most 15%.

【００１５】ＭｇＯ、ＣａＯ、ＳｒＯおよびＢａＯの内
の１種以上を含有する場合、その含有量の合計は３５％
以下であることが好ましい。３５％超では軟化点が高く
なりすぎるおそれがある。より好ましくは１９％以下、
特に好ましくは１５％以下である。また、前記含有量の
合計は２％以上であることが好ましい。２％未満では、
ガラスが不安定になるおそれがある、または焼成時に結
晶が析出しやすくなるおそれがある。より好ましくは
２．５％以上、特に好ましくは４％以上、最も好ましく
は８％以上である。When one or more of MgO, CaO, SrO and BaO are contained, the total content thereof is 35%
The following is preferred. If it exceeds 35%, the softening point may be too high. More preferably 19% or less,
Especially preferably, it is 15% or less. Further, the total content is preferably 2% or more. If less than 2%,
The glass may become unstable, or crystals may be easily precipitated during firing. It is more preferably at least 2.5%, particularly preferably at least 4%, most preferably at least 8%.

【００１６】Ａｌ2Ｏ3、Ｉｎ2Ｏ3およびＷＯ3はいずれ
も必須ではないが、化学的耐久性を高くするために、ま
たは焼成時の結晶化を抑制するために、それぞれ１０％
まで含有してもよい。１０％超では軟化点が高くなりす
ぎるおそれがある。より好ましくは５％以下、特に好ま
しくは４％以下である。Al 2 O 3 , In 2 O 3 and WO 3 are not essential, but are each 10% in order to increase chemical durability or suppress crystallization during firing.
May be contained. If it exceeds 10%, the softening point may be too high. It is more preferably at most 5%, particularly preferably at most 4%.

【００１７】Ａｌ2Ｏ3、Ｉｎ2Ｏ3およびＷＯ3の内の１
種以上を含有する場合、その含有量の合計は０．５〜１
０％の範囲にあることが好ましい。１０％超では軟化点
が高くなりすぎるおそれがある。より好ましくは７％以
下、特に好ましくは５％以下である。One of Al 2 O 3 , In 2 O 3 and WO 3
When containing more than one species, the total content is 0.5 to 1
It is preferably in the range of 0%. If it exceeds 10%, the softening point may be too high. It is more preferably at most 7%, particularly preferably at most 5%.

【００１８】Ｌｉ2Ｏ、Ｎａ2ＯおよびＫ2Ｏはいずれも
必須ではないが、軟化点を低下させるためにそれぞれ３
％まで含有してもよい。３％超では電気絶縁性が低下す
るおそれがある、化学的耐久性が低下するおそれがあ
る、または膨張係数が大きくなりすぎるおそれがある。
より好ましくは１％以下、特に好ましくは０．５％以下
である。Ｌｉ2Ｏ、Ｎａ2ＯおよびＫ2Ｏのいずれも実質
的に含有しないこと、すなわち不純物レベル以下である
ことが最も好ましい。Although Li 2 O, Na 2 O and K 2 O are not essential, they are each 3 to reduce the softening point.
%. If it exceeds 3%, the electrical insulation may be reduced, the chemical durability may be reduced, or the coefficient of expansion may be too large.
It is more preferably at most 1%, particularly preferably at most 0.5%. Most preferably, it does not substantially contain any of Li 2 O, Na 2 O and K 2 O, that is, it is at most an impurity level or less.

【００１９】Ｌｉ2Ｏ、Ｎａ2ＯおよびＫ2Ｏの含有量の
合計は３％以下であることが好ましい。３％超では電気
絶縁性が低下するおそれがある、化学的耐久性が低下す
るおそれがある、または膨張係数が大きくなりすぎるお
それがある。より好ましくは１％以下、特に好ましくは
０．５％以下である。The total content of Li 2 O, Na 2 O and K 2 O is preferably at most 3%. If it exceeds 3%, the electrical insulation may be reduced, the chemical durability may be reduced, or the coefficient of expansion may be too large. It is more preferably at most 1%, particularly preferably at most 0.5%.

【００２０】本発明のガラスは実質的に上記成分からな
るが、これ以外の成分を合計で５モル％まで含有しても
よい。このような成分として、Ｌａ2Ｏ3、ＣｅＯ2、等
の希土類酸化物、ＳｉＯ2、ＴｉＯ2、Ｖ2Ｏ5、ＭｎＯ、
Ｆｅ2Ｏ3、ＣｏＯ、ＮｉＯ、ＣｕＯ、Ｙ2Ｏ3、Ｚｒ
Ｏ2、ＭｏＯ3、Ｒｈ2Ｏ3、ＰｄＯ、Ａｇ2Ｏ、ＴｅＯ2、
Ｂｉ2Ｏ3が例示される。なお、ＰｂＯおよびＣｄＯにつ
いてはいずれも実質的に含有しない、すなわち不純物レ
ベル以下である。The glass of the present invention consists essentially of the above components, but may contain other components up to 5 mol% in total. Such components include rare earth oxides such as La 2 O 3 and CeO 2 , SiO 2 , TiO 2 , V 2 O 5 , MnO,
Fe 2 O 3 , CoO, NiO, CuO, Y 2 O 3 , Zr
O 2 , MoO 3 , Rh 2 O 3 , PdO, Ag 2 O, TeO 2 ,
Bi 2 O 3 is exemplified. It should be noted that PbO and CdO are substantially not contained, that is, they are lower than the impurity level.

【００２１】また、Ｆ、Ｃｌ、等のハロゲン元素も実質
的に含有しないことが好ましい。ハロゲン元素は焼成時
にガス化し、ＰＤＰ、ＶＦＤ、等における蛍光体と反応
して蛍光体を劣化させたり、また、ＶＦＤのフィラメン
トに付着してエミッション低下を起したりするおそれが
あるからである。Further, it is preferable that halogen elements such as F and Cl are not substantially contained. This is because the halogen element gasifies during firing and may react with the phosphor in PDPs, VFDs, and the like to degrade the phosphor, or adhere to VFD filaments to cause a reduction in emission.

【００２２】本発明のガラスフリットは本発明のガラス
の粉末を含有し、この他に、低膨張セラミックスフィラ
ー、耐熱顔料の内の少なくとも一方を含有する。ここで
いう低膨張セラミックスフィラーは、膨張係数が７０×
１０-7／℃以下であるセラミックスフィラーであり、ア
ルミナ、ムライト、ジルコン、コーディエライト、チタ
ン酸アルミニウム、β−スポデュメン、α−石英、β−
石英固溶体およびβ−ユークリプタイトから選ばれる１
種以上の粉末であることが、取り扱いやすさまたは入手
しやすさの点から好ましい。また、耐熱顔料として、た
とえばチタニア等の白色顔料、Ｆｅ−Ｍｎ複酸化物系、
Ｆｅ−Ｃｏ−Ｃｒ複酸化物系、Ｆｅ−Ｍｎ−Ａｌ複酸化
物系等の黒色顔料が挙げられる。The glass frit of the present invention contains the powder of the glass of the present invention, and further contains at least one of a low expansion ceramic filler and a heat-resistant pigment. The low expansion ceramic filler here has an expansion coefficient of 70 ×
A ceramic filler having a temperature of 10 −7 / ° C. or less, alumina, mullite, zircon, cordierite, aluminum titanate, β-spodumene, α-quartz, β-
1 selected from quartz solid solution and β-eucryptite
More than one kind of powder is preferable from the viewpoint of easy handling or availability. As the heat-resistant pigment, for example, white pigments such as titania, Fe-Mn double oxide,
Black pigments such as Fe-Co-Cr double oxides and Fe-Mn-Al double oxides are exemplified.

【００２３】本発明のガラスフリットを焼成して得られ
る焼成物の膨張係数は６０×１０-7〜９０×１０-7／℃
の範囲にあることが好ましい。膨張係数がこの範囲外で
は焼成物と下地のガラスとの膨張マッチングが困難にな
るおそれがある。The coefficient of expansion of the fired product obtained by firing the glass frit of the present invention is 60 × 10 −7 to 90 × 10 −7 / ° C.
Is preferably within the range. If the expansion coefficient is out of this range, expansion matching between the fired material and the underlying glass may be difficult.

【００２４】次に本発明のガラスフリットの組成につい
て説明する。本発明のガラスの粉末は必須である。その
含有量は５０〜９９．９体積％であることが好ましい。
５０体積％未満ではガラスフリットの焼成時の流動性が
小さくなりすぎるおそれがある。より好ましくは５５体
積％以上、特に好ましくは６０体積％以上である。ま
た、その含有量が９９．９体積％超では、低膨張セラミ
ックスフィラーまたは耐熱顔料の含有量が小さくなりす
ぎる。より好ましくは９９体積％以下、特に好ましくは
９８体積％以下である。Next, the composition of the glass frit of the present invention will be described. The powder of the glass of the present invention is essential. The content is preferably 50 to 99.9% by volume.
If it is less than 50% by volume, the fluidity of the glass frit during firing may be too small. It is more preferably at least 55% by volume, particularly preferably at least 60% by volume. On the other hand, when the content exceeds 99.9% by volume, the content of the low expansion ceramic filler or the heat-resistant pigment becomes too small. It is more preferably at most 99% by volume, particularly preferably at most 98% by volume.

【００２５】低膨張セラミックスフィラーは、膨張係数
を小さくするために５０体積％まで含有してもよい。５
０体積％超では焼成時の流動性が小さくなりすぎるおそ
れがある。より好ましくは４５体積％以下、特に好まし
くは４０体積％以下である。また、低膨張セラミックス
フィラーを含有する場合はその含有量は１体積％以上で
あることがより好ましく、２体積％以上であることが特
に好ましい。耐熱顔料は、必要に応じて４０体積％まで
含有してもよい。４０体積％超では焼成時の流動性が小
さくなりすぎるおそれがある。The low expansion ceramic filler may be contained up to 50% by volume in order to reduce the expansion coefficient. 5
If it exceeds 0% by volume, the fluidity during firing may be too small. It is more preferably at most 45% by volume, particularly preferably at most 40% by volume. When the low-expansion ceramic filler is contained, the content is more preferably 1% by volume or more, and particularly preferably 2% by volume or more. The heat-resistant pigment may be contained up to 40% by volume as necessary. If it exceeds 40% by volume, the fluidity during firing may be too small.

【００２６】本発明のガラスフリットは低膨張セラミッ
クスフィラー、耐熱顔料の内の少なくともいずれか一方
を含有しなければならないが、それらの含有量の合計は
０．１〜５０体積％であることが好ましい。より好まし
くは１〜４５体積％、特に好ましくは２〜４０体積％で
ある。The glass frit of the present invention must contain at least one of a low-expansion ceramic filler and a heat-resistant pigment, and the total content thereof is preferably 0.1 to 50% by volume. . It is more preferably 1 to 45% by volume, particularly preferably 2 to 40% by volume.

【００２７】本発明のガラスフリットは、通常はビヒク
ルと混合してガラスペーストとされる。ビヒクルとの混
合は、乳鉢、三本ロール、等を用いて行われる。このガ
ラスペーストをスクリーン印刷等の方法により下地のガ
ラス、たとえばガラス基板またはガラス基板上に形成さ
れた薄膜の所定部位に塗布し、たとえば６００℃以下で
焼成し、封着、被覆、隔壁形成、等を行う。前記ビヒク
ルとしては、エチルセルロース、ニトロセルロース、等
の樹脂を、α−テルピネオール、ブチルカルビトールア
セテート、酢酸イソペンチル、等の溶剤に溶解したもの
が通常用いられる。The glass frit of the present invention is usually mixed with a vehicle to form a glass paste. Mixing with the vehicle is performed using a mortar, a three-roll mill, or the like. The glass paste is applied to a predetermined portion of an underlying glass, for example, a glass substrate or a thin film formed on the glass substrate, by a method such as screen printing, and baked at, for example, 600 ° C. or less, and sealing, coating, partition wall formation, and the like are performed. I do. As the vehicle, those obtained by dissolving a resin such as ethyl cellulose or nitrocellulose in a solvent such as α-terpineol, butyl carbitol acetate, or isopentyl acetate are generally used.

【００２８】[0028]

【実施例】表のＰ2Ｏ5〜ＷＯ3の欄にモル％表示で示し
た組成となるように原料を調合、混合して蓋付きの石英
ルツボに入れ、１１００℃に加熱し３０分間溶融した。
次いで、溶融ガラスをステンレス製ローラに流し込んで
フレーク化した。得られたフレーク状のガラスをアルミ
ナ製ボールミルで１０５分間粉砕してガラス粉末とし
た。EXAMPLES Raw materials were prepared and mixed so as to have the composition indicated by mol% in the column of P 2 O 5 to WO 3 in the table, put into a quartz crucible with a lid, and heated to 1100 ° C. and melted for 30 minutes. did.
Next, the molten glass was poured into a stainless steel roller to form flakes. The obtained flaky glass was pulverized with an alumina ball mill for 105 minutes to obtain glass powder.

【００２９】得られたガラス粉末について、ガラス転移
点Ｔg（単位：℃）、軟化点Ｔs（単位：℃）、結晶化ピ
ーク温度Ｔc（単位：℃）、膨張係数α（単位：１０-7
／℃）、溶出量Ｑd（％）、フローボタン径Ｄ（単位：
ｍｍ）、フローボタン外観、を測定・評価した。その方
法を以下に、結果を表に示す。例１〜５は５６０℃での
焼成に好適な実施例、例６、７は５８０℃での焼成に好
適な実施例、例８は比較例である。With respect to the obtained glass powder, glass transition point T g (unit: ° C.), softening point T s (unit: ° C.), crystallization peak temperature T c (unit: ° C.), expansion coefficient α (unit: 10) -7
/ ° C), elution amount Q d (%), flow button diameter D (unit:
mm) and flow button appearance were measured and evaluated. The method is described below, and the results are shown in the table. Examples 1 to 5 are examples suitable for firing at 560 ° C, Examples 6 and 7 are examples suitable for firing at 580 ° C, and Example 8 is a comparative example.

【００３０】ガラス転移点、軟化点、結晶化ピーク温
度：平均粒径が１０〜２０μｍのガラス粉末を試料とし
て示差熱分析により昇温速度１０℃／分で室温から８０
０℃までの範囲で測定した。なお、アルミナ粉末を標準
物質とした。５６０℃で焼成する場合は、軟化点が５６
０℃以下かつ結晶化ピーク温度が６２０℃以上であるこ
とが好ましい。５８０℃で焼成する場合は、軟化点が５
８０℃以下かつ結晶化ピーク温度が６５０℃以上である
ことが好ましい。Glass transition point, softening point, crystallization peak temperature: A glass powder having an average particle size of 10 to 20 μm was used as a sample, and the temperature was raised from room temperature to 80 ° C. at a heating rate of 10 ° C./min.
It was measured in the range up to 0 ° C. Alumina powder was used as a standard substance. When firing at 560 ° C., the softening point is 56
It is preferable that the crystallization peak temperature is 0 ° C or lower and the crystallization peak temperature is 620 ° C or higher. When firing at 580 ° C., the softening point is 5
It is preferable that the crystallization peak temperature is not higher than 650 ° C and not higher than 80 ° C.

【００３１】膨張係数：前記溶融ガラスをステンレス製
板の上に流し出し、ガラス転移点近傍で徐冷した。徐冷
したガラスを直径２ｍｍ、長さ２０ｍｍの棒状に加工し
たものを試料とし、石英ガラスを標準試料として、示差
熱膨張計により５０〜２５０℃の範囲における平均線膨
張係数を測定した。Expansion coefficient: The molten glass was poured onto a stainless steel plate and gradually cooled near the glass transition point. A sample obtained by processing the slowly cooled glass into a rod having a diameter of 2 mm and a length of 20 mm was used as a sample, and the average linear expansion coefficient in the range of 50 to 250 ° C. was measured with a differential thermal dilatometer using quartz glass as a standard sample.

【００３２】溶出量：膨張係数測定用試料と同じ試料を
８０℃の水に２４時間浸漬し、浸漬前後の試料重量から
重量減少率を算出し、％表示とした。この溶出量は化学
的耐久性の指標であり、０．１％以下であることが好ま
しく、０．０２％以下であることがより好ましく、０．
０１％未満であることが特に好ましい。Elution amount: The same sample as the sample for measuring the expansion coefficient was immersed in water at 80 ° C. for 24 hours, and the weight loss rate was calculated from the weight of the sample before and after immersion, and expressed as%. This elution amount is an index of chemical durability, and is preferably 0.1% or less, more preferably 0.02% or less, and 0.1% or less.
Particularly preferred is less than 01%.

【００３３】フローボタン径：ガラス粉末３．５ｇを直
径１２．７ｍｍの円柱状に加圧成形したものを試料とし
た。この試料を、例１〜５および例８については５６０
℃に１０分間、例６、７については５８０℃に１０分
間、それぞれ保持した。この加熱処理後の試料の直径を
測定した。この直径は１３ｍｍ以上であることが好まし
く、１４ｍｍ以上であることがより好ましい。Flow button diameter: A sample was prepared by pressing 3.5 g of glass powder into a columnar shape having a diameter of 12.7 mm. This sample was 560 for Examples 1-5 and 8
C. for 10 minutes and for Examples 6 and 7 at 580.degree. C. for 10 minutes. The diameter of the sample after the heat treatment was measured. This diameter is preferably at least 13 mm, more preferably at least 14 mm.

【００３４】フローボタン外観：フローボタン径の測定
によって得られた前記加熱処理後の試料の外観を観察し
た。光沢があることが好ましい。光沢があるものを○、
光沢がないものを×、でそれぞれ示した。なお、例８の
ガラスの粉末は前記加熱処理によっては充分焼結しなか
った。Flow button appearance: The appearance of the sample after the heat treatment obtained by measuring the flow button diameter was observed. It is preferably glossy. ○, glossy
Those having no gloss are indicated by x. The glass powder of Example 8 was not sufficiently sintered by the heat treatment.

【００３５】[0035]

【表１】 [Table 1]

【００３６】[0036]

【発明の効果】本発明のガラスを用いることにより、Ｐ
ＤＰ、ＶＦＤ、等における封着、被覆、隔壁形成、等に
使用できる焼成物が得られる。また、電気絶縁性にも優
れているので電気的な問題がおこりにくい。By using the glass of the present invention, P
A fired product that can be used for sealing, coating, partition wall formation, and the like in DP, VFD, and the like is obtained. In addition, since it has excellent electrical insulation, electrical problems are unlikely to occur.

フロントページの続き Ｆターム(参考） 4G062 AA08 AA09 AA15 BB09 CC10 DA01 DB01 DB02 DB03 DC02 DC03 DC04 DD04 DD05 DE03 DE04 DE05 DF01 EA01 EA02 EA03 EA10 EB01 EB02 EB03 EC01 EC02 EC03 ED01 ED02 ED03 ED04 ED05 EE01 EE02 EE03 EE04 EE05 EF01 EF02 EF03 EF04 EF05 EG01 EG02 EG03 EG04 EG05 FA01 FB01 FC01 FD01 FE03 FE04 FE05 FF01 FG01 FH01 FJ01 FK01 FL01 GA01 GA10 GB01 GC01 GD01 GE01 HH01 HH03 HH05 HH06 HH07 HH08 HH09 HH11 HH13 HH15 HH17 HH20 JJ01 JJ03 JJ05 JJ07 JJ10 KK01 KK03 KK05 KK07 KK10 MM07 MM10 NN26 NN30 NN32 PP01 PP02 PP03 PP04 PP05 PP06 PP09 PP13 PP16 5G303 AA07 AB01 BA12 CA02 CB01 CB02 CB03 CB06 CB14 CB16 CB17 CB20 CB24 CB31 CB32 CB37 CB38 CB43 Continued on the front page F-term (reference) 4G062 AA08 AA09 AA15 BB09 CC10 DA01 DB01 DB02 DB03 DC02 DC03 DC04 DD04 DD05 DE03 DE04 DE05 DF01 EA01 EA02 EA03 EA10 EB01 EB02 EB03 EC01 EC02 EC03 ED01 ED02 EE03 EE03 ED04 EF03 EF04 EF05 EG01 EG02 EG03 EG04 EG05 FA01 FB01 FC01 FD01 FE03 FE04 FE05 FF01 FG01 FH01 FJ01 FK01 FL01 GA01 GA10 GB01 GC01 GD01 GE01 H07 KK01 GH01 H07 KK MM10 NN26 NN30 NN32 PP01 PP02 PP03 PP04 PP05 PP06 PP09 PP13 PP16 5G303 AA07 AB01 BA12 CA02 CB01 CB02 CB03 CB06 CB14 CB16 CB17 CB20 CB24 CB31 CB32 CB37 CB38 CB43

Claims (2)

【特許請求の範囲】[Claims] 【請求項１】下記酸化物基準のモル％表示で、 Ｐ2Ｏ5 １５〜５０、 ＳｎＯ ２〜３５、 ＺｎＯ ５〜４５、 Ｂ2Ｏ3 ０．１〜３０、 ＭｇＯ ０〜３５、 ＣａＯ ０〜３５、 ＳｒＯ ０〜３５、 ＢａＯ ０〜３５、 Ａｌ2Ｏ3 ０〜１０、 Ｉｎ2Ｏ3 ０〜１０、 ＷＯ3 ０〜１０、 Ｌｉ2Ｏ ０〜３、 Ｎａ2Ｏ ０〜３、 Ｋ2Ｏ ０〜３、 から実質的になり、ＭｇＯ＋ＣａＯ＋ＳｒＯ＋ＢａＯが
０〜３５モル％であり、Ａｌ2Ｏ3＋Ｉｎ2Ｏ3＋ＷＯ3が
０〜１０モル％であり、Ｌｉ2Ｏ＋Ｎａ2Ｏ＋Ｋ2Ｏが０
〜３モル％であり、かつ、ＳｎＯのＺｎＯに対するモル
比が１未満である無鉛低融点ガラス。1. The following oxide-based molar percentages are represented by: P 2 O 5 15 to 50, SnO 2 to 35, ZnO 5 to 45, B 2 O 3 0.1 to 30, MgO 0 to 35, CaO 0 ~35, SrO 0~35, BaO 0~35, Al 2 O 3 0~10, In 2 O 3 0~10, WO 3 0~10, Li 2 O 0~3, Na 2 O 0~3, K 2 O 0 to 3, essentially made from, MgO + CaO + SrO + BaO is 0 to 35 mol%, Al 2 O 3 + in 2 O 3 + WO 3 is 0 to 10 mol%, Li 2 O + Na 2 O + K 2 O is 0
A lead-free low-melting glass having a molar ratio of SnO to ZnO of less than 1 by 3 mol%. 【請求項２】低膨張セラミックスフィラーおよび耐熱顔
料の少なくともいずれか一方と、請求項１に記載の無鉛
低融点ガラスの粉末を含有するガラスフリット。2. A glass frit containing at least one of a low-expansion ceramic filler and a heat-resistant pigment, and the powder of the lead-free low-melting glass according to claim 1.
JP31562299A 1999-11-05 1999-11-05 Lead-free low melting glass and glass frit Expired - Fee Related JP4061792B2 (en)

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