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JP3814810B2 - Bismuth glass composition - Google Patents

Bismuth glass composition Download PDF

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Publication number
JP3814810B2
JP3814810B2 JP11022096A JP11022096A JP3814810B2 JP 3814810 B2 JP3814810 B2 JP 3814810B2 JP 11022096 A JP11022096 A JP 11022096A JP 11022096 A JP11022096 A JP 11022096A JP 3814810 B2 JP3814810 B2 JP 3814810B2
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Prior art keywords
glass
content
glass composition
thermal expansion
bismuth
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JPH09278483A (en
Inventor
俊郎 山中
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/14—Silica-free oxide glass compositions 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
    • 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
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders

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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)

Description

【０００１】
【産業上の利用分野】
本発明は電子部品の接着、封着、被覆等に好適なビスマス系ガラス組成物に関するものである。
【０００２】
【従来の技術】
従来から電子部品の接着や封着材料として、或いは電子部品に形成された電極や抵抗体の保護や絶縁のための被覆材料としてガラスが用いられている。
【０００３】
これらのガラスは、その用途に応じて化学耐久性、機械的強度、流動性、電気絶縁性等種々の特性が要求されるが、何れの用途にも共通する特性として、低温で焼成可能であることが挙げられる。それゆえ何れの用途においても、ガラスの融点を下げる効果が極めて大きいＰｂＯを多量に含有した低融点ガラスが広く用いられている。
【０００４】
【発明が解決しようとする課題】
しかしながら最近、ＰｂＯ含有ガラスに対して環境上の問題が指摘されており、ＰｂＯを含まないガラスに置換することが望まれている。またＰｂＯを多量に含有するガラスを用いて電気絶縁膜を形成すると、Ｐｂ2+イオンが拡散して電気絶縁性が低下し易いという不都合もある。
【０００５】
本発明は上記事情に鑑みなされたものであり、６５０℃以下の温度で焼成が可能であるとともに、ＰｂＯを含有しないために環境問題が生じたり、電気絶縁性が低下する恐れがないガラス組成物を提供することを目的とする。
【０００６】
【課題を解決するための手段】
本発明のビスマス系ガラス組成物は、重量百分率でＢｉ2Ｏ3 ２０〜８０％、Ｂ2Ｏ3 ５〜３５％、ＢａＯ ０〜３５％、ＳｒＯ ０〜３０％、ＢａＯ＋ＳｒＯ ５〜４０％（ただし５％を含まず）、ＺｎＯ ０〜９％、ＣａＯ ０〜１０％、Ｆｅ2Ｏ3 ０〜５％、ＣｕＯ ２〜１０％、ＺｎＯ＋ＣａＯ＋Ｆｅ2Ｏ3＋ＣｕＯ ２〜２０％、ＳｉＯ2 ０〜８％、Ａｌ2Ｏ3 ０〜５％、Ｃｓ2Ｏ ０〜５％、Ｆ2 ０〜５％の組成を有し、本質的にＰｂＯを含有しないことを特徴とする。
【０００７】
【作用】
本発明のビスマス系ガラス組成物の組成を上記のように限定した理由は次のとおりである。
【０００８】
Ｂｉ2 Ｏ3 はガラスの軟化点を下げるための主要成分であり、その含有量は２０〜８０％、好ましくは４０〜７５％である。Ｂｉ2 Ｏ3 の含有量が２０％より少ないと軟化点が高くなり過ぎて６５０℃以下で焼成できなくなり、８０％より多いと熱膨張係数が大きくなり過ぎて好ましくない。
【０００９】
Ｂ2 Ｏ3 はガラス形成成分として必須であり、その含有量は５〜３５％、好ましくは７〜２５％である。Ｂ2 Ｏ3 の含有量が５％より少ないとガラスが不安定になって失透し易くなる。また失透を生じない場合でも、焼成時に結晶の析出速度が極めて大きく、接着、封着、被覆等の作業に必要な流動性が得られない。一方、Ｂ2 Ｏ3 が３５％より多くなるとガラスの粘性が高くなり過ぎて６５０℃以下の温度で焼成が困難になる。
【００１０】
ＢａＯとＳｒＯはガラスの安定化に大きな効果があり、これらを合量で５〜４０％（ただし５％を含まず）、好ましくは７〜３０％含有する。これらの成分の合量が５％以下であればその効果がなく、一方、４０％より多くなると逆に安定なガラスが得られなくなる。またＢａＯの含有量は０〜３５％、好ましくは０〜２５％、ＳｒＯの含有量は０〜３０％、好ましくは０〜２０％である。ＢａＯ及びＳｒＯがそれぞれその範囲を超えると安定なガラスが得られなくなる。
【００１１】
ＺｎＯ、ＣａＯ、Ｆｅ2Ｏ3及びＣｕＯは何れもガラスを安定化させるための成分であり、その含有量は合量で２〜２０％、好ましくは２〜１５％である。これらの成分が合量で２％より少ないとその効果がなく、２０％より多いと逆にガラスが不安定になる。またＺｎＯの含有量は０〜９％、好ましくは０．１〜９％、ＣａＯの含有量は０〜１０％、好ましくは０〜５％、Ｆｅ2Ｏ3の含有量は０〜５％、好ましくは０〜４％、ＣｕＯの含有量は２〜１０％、好ましくは２〜５％である。各成分の含有量が上記範囲を超えると逆に安定なガラスが得られなくなる。
【００１２】
ＳｉＯ2 及びＡｌ2 Ｏ3 は何れもガラスをより安定化させるために含有させる成分であり、ＳｉＯ2 の含有量は０〜８％、好ましくは０〜５％、Ａｌ2 Ｏ3 の含有量は０〜５％、好ましくは０〜４％である。これらの成分が上記範囲を超えるとガラスの粘性が高くなり過ぎたり、失透し易くなって好ましくない。
【００１３】
Ｃｓ2 ＯとＦ2 はガラスをより低粘性化する成分であり、Ｃｓ2 Ｏの含有量は０〜５％、好ましくは０〜３％、Ｆ2 の含有量は０〜５％、好ましくは０〜２％である。これらの成分が上記範囲を超えるとガラスの化学耐久性が低下する。
【００１４】
なお上記成分以外にも、ガラスの粘性や熱膨張係数の調整のために、ＭｇＯ、Ｌａ2 Ｏ3 、ＴｉＯ2 、ＺｒＯ2 、Ｖ2 Ｏ5 、Ｎｂ2 Ｏ5 、ＭｏＯ3 、ＷＯ3 、Ａｇ2 Ｏ、Ｎａ2 Ｏ、Ｋ2 Ｏ、Ｌｉ2 Ｏ等を５％以下添加することが可能である。
【００１５】
以上の組成を有するガラスは、ガラス転移点が約５００℃以下であり、良好な流動性を示す非結晶性又は結晶性のガラスである。また３０〜３００℃における熱膨張係数が約８０×１０-7／℃以上であり、これと適合する高膨張材料を６５０℃以下の温度で接着、封着又は被覆することが可能である。
【００１６】
一方、熱膨張係数の適合しない材料の接着、封着又は被覆を行う場合、対象物との熱膨張係数差を是正するために、耐火性フィラーを混合して使用することが可能である。また機械的強度が不足する場合も耐火性フィラーを混合して使用することができる。
【００１７】
耐火性フィラーを混合する場合、その混合割合はガラス４５〜９５体積％と耐火性フィラー５５〜５体積％であることが好ましい。両者の割合をこのように限定した理由は、耐火性フィラーが５体積％より少ないとその効果がなく、５５体積％より多くなると流動性が悪くなるためである。
【００１８】
耐火性フィラーとしては、チタン酸鉛系セラミック、ウイレマイト系セラミック、β−ユークリプタイト、コーディエライト、ジルコン系セラミック、酸化錫系セラミック、ムライト、石英ガラス、アルミナ等の粉末を単独、或は組み合わせて使用することが好ましい。
【００１９】
なお本発明のビスマス系ガラス組成物の具体的な用途としては、▲１▼蛍光表示管−パッケージの封着、絶縁層の形成、▲２▼プラズマディスプレイ−パネルの気密封着、絶縁層や誘電体層の形成、バリアリブの形成、▲３▼磁気ヘッド−コア同士又はコアとスライダーの封着、等が挙げられる。また使用時の形態は特に制限はなく、粉末状、板状、棒状等、その用途に応じて種々の形態に成形して使用すればよい。
【００２０】
【実施例】
以下、本発明のビスマス系低融点ガラス組成物を実施例に基づいて詳細に説明する。
【００２１】
表１及び表２は、本発明の実施例（試料Ｎｏ．２、５及び１０）を示すものである。なおその他の試料は参考例である。
【００２２】
【表１】

Figure 0003814810
【００２３】
【表２】
Figure 0003814810
【００２４】
表の各試料は次のようにして調製した。
【００２５】
まず表に示したガラス組成となるように各種酸化物、炭酸塩等を調合したガラスバッチを準備し、これを白金坩堝に入れて９００〜１１００℃で２時間溶融した後、溶融ガラスをステンレス製の金型に流しだし成形した。得られた各試料について、ガラス転移点、３０〜３００℃における熱膨張係数、焼成温度、及び結晶性か非結晶性かを評価した。結果を表に示す。
【００２６】
表から明らかなように、実施例の各試料は、ガラス転移点が３９０〜４５２℃、３０〜３００℃の温度範囲における熱膨張係数が９０〜１１０×１０-7／℃であり、焼成温度が６００℃以下であった。また試料Ｎｏ．２は非結晶性、Ｎｏ．５及びＮｏ．１０は結晶性であった。
【００２７】
なお転移点は示差熱分析装置（ＤＴＡ）により求めた。熱膨張係数は、成形したガラス体を直径４ｍｍ、長さ４０ｍｍの円柱状に研磨加工し、押し棒式熱膨張係数測定装置を用いて測定した。焼成温度は、次のようにして求めた。まずガラス体を粉砕してガラス粉末を得、ガラスの真比重に相当する重量のガラス粉末を金型を用いて外径２０ｍｍ、高さ約５ｍｍのボタン状に加圧成形した。次いでこのボタンを板ガラスの上に載せて電気炉に入れ、１０℃／分の速度で昇温し、種々の温度で１０分間保持した。このようにして得られたボタンの外径が２１〜２２ｍｍの範囲にある温度を焼成温度とした。また結晶性か非結晶性かの判定は、焼成温度で１０分間加熱された後の試料の外観を顕微鏡で観察し、結晶の析出状態から評価した。
【００２８】
【発明の効果】
以上のように本発明のビスマス系ガラス組成物は、ＰｂＯを含有しないため、環境問題を引き起こす心配がない。また６５０℃以下の温度で焼成できるため、従来のＰｂＯを含有する低融点ガラスの代替材料として、電子部品の接着、封着、被覆等の用途に使用することが可能である。[0001]
[Industrial application fields]
The present invention relates to a bismuth-based glass composition suitable for bonding, sealing, coating, etc. of electronic components.
[0002]
[Prior art]
Conventionally, glass has been used as an adhesive or sealing material for electronic components, or as a coating material for protecting and insulating electrodes and resistors formed on electronic components.
[0003]
These glasses are required to have various properties such as chemical durability, mechanical strength, fluidity, and electrical insulation depending on the application, but can be fired at a low temperature as a property common to all applications. Can be mentioned. Therefore, in any application, a low melting point glass containing a large amount of PbO that has a great effect of lowering the melting point of the glass is widely used.
[0004]
[Problems to be solved by the invention]
Recently, however, environmental problems have been pointed out with respect to PbO-containing glasses, and it is desired to replace them with glasses that do not contain PbO. In addition, when an electrical insulating film is formed using glass containing a large amount of PbO, there is also a disadvantage that Pb 2+ ions diffuse and electrical insulating properties are likely to be lowered.
[0005]
The present invention has been made in view of the above circumstances, and can be fired at a temperature of 650 ° C. or lower, and does not contain PbO, so that there is no risk of environmental problems or a decrease in electrical insulation. The purpose is to provide.
[0006]
[Means for Solving the Problems]
The bismuth-based glass composition of the present invention is, by weight percentage, Bi 2 O 3 20-80%, B 2 O 3 5-35%, BaO 0-35%, SrO 0-30%, BaO + SrO 5-40% (however, 5% free of), ZnO 0~9%, CaO 0~10 %, Fe 2 O 3 0~5%, CuO 2 ~10%, ZnO + CaO + Fe 2 O 3 + CuO 2 ~20%, SiO 2 0~8% , Al 2 O 3 0 to 5%, Cs 2 O 0 to 5%, F 2 0 to 5%, and essentially free of PbO.
[0007]
[Action]
The reason for limiting the composition of the bismuth-based glass composition of the present invention as described above is as follows.
[0008]
Bi 2 O 3 is a main component for lowering the softening point of the glass, and its content is 20 to 80%, preferably 40 to 75%. If the content of Bi 2 O 3 is less than 20%, the softening point becomes too high and it becomes impossible to fire at 650 ° C. or less, and if it exceeds 80%, the thermal expansion coefficient becomes too large.
[0009]
B 2 O 3 is essential as a glass forming component, and its content is 5 to 35%, preferably 7 to 25%. If the content of B 2 O 3 is less than 5%, the glass becomes unstable and tends to devitrify. Even when devitrification does not occur, the crystal deposition rate is extremely high during firing, and the fluidity necessary for operations such as adhesion, sealing, and coating cannot be obtained. On the other hand, if B 2 O 3 exceeds 35%, the viscosity of the glass becomes too high and firing at a temperature of 650 ° C. or less becomes difficult.
[0010]
BaO and SrO have a great effect on the stabilization of the glass, and these are contained in a total amount of 5 to 40% (excluding 5%) , preferably 7 to 30%. If the total amount of these components is 5% or less, the effect is not obtained. On the other hand, if it exceeds 40%, a stable glass cannot be obtained. The content of BaO is 0 to 35%, preferably 0 to 25%, and the content of SrO is 0 to 30%, preferably 0 to 20%. If BaO and SrO exceed the respective ranges, stable glass cannot be obtained.
[0011]
ZnO, CaO, Fe 2 O 3 and CuO is a component for stabilizing the glass any, its content is 2-20% in total, preferably 2 15%. If the total amount of these components is less than 2 %, the effect is not obtained, and if it exceeds 20%, the glass becomes unstable. The ZnO content is 0 to 9%, preferably 0.1 to 9%, the CaO content is 0 to 10%, preferably 0 to 5%, and the Fe 2 O 3 content is 0 to 5%. Preferably it is 0 to 4%, and the content of CuO is 2 to 10%, preferably 2 to 5%. If the content of each component exceeds the above range, a stable glass cannot be obtained.
[0012]
SiO 2 and Al 2 O 3 are both components that are added to stabilize the glass. The content of SiO 2 is 0 to 8%, preferably 0 to 5%, and the content of Al 2 O 3 is 0 to 5%, preferably 0 to 4%. If these components exceed the above range, the viscosity of the glass becomes too high or the glass tends to devitrify, which is not preferable.
[0013]
Cs 2 O and F 2 are components that lower the viscosity of the glass. The content of Cs 2 O is 0 to 5%, preferably 0 to 3%, and the content of F 2 is 0 to 5%, preferably 0-2%. When these components exceed the above range, the chemical durability of the glass is lowered.
[0014]
In addition to the above components, MgO, La 2 O 3 , TiO 2 , ZrO 2 , V 2 O 5 , Nb 2 O 5 , MoO 3 , WO 3 , Ag are used for adjusting the viscosity and thermal expansion coefficient of glass. It is possible to add 5% or less of 2 O, Na 2 O, K 2 O, Li 2 O and the like.
[0015]
The glass having the above composition is an amorphous or crystalline glass having a glass transition point of about 500 ° C. or less and showing good fluidity. Further, the coefficient of thermal expansion at 30 to 300 ° C. is about 80 × 10 −7 / ° C. or higher, and a high expansion material compatible therewith can be bonded, sealed or coated at a temperature of 650 ° C. or lower.
[0016]
On the other hand, when bonding, sealing, or coating a material that does not match the thermal expansion coefficient, it is possible to mix and use a refractory filler in order to correct the difference in thermal expansion coefficient from the object. Also, when the mechanical strength is insufficient, a refractory filler can be mixed and used.
[0017]
When mixing a refractory filler, the mixing ratio is preferably 45 to 95% by volume of glass and 55 to 5% by volume of refractory filler. The reason for limiting the ratio of the two in this way is that when the refractory filler is less than 5% by volume, the effect is not achieved, and when it exceeds 55% by volume, the fluidity is deteriorated.
[0018]
As the refractory filler, powders of lead titanate ceramics, willemite ceramics, β-eucryptite, cordierite, zircon ceramics, tin oxide ceramics, mullite, quartz glass, alumina, etc., alone or in combination Are preferably used.
[0019]
Specific applications of the bismuth-based glass composition of the present invention include (1) fluorescent display tube-sealing of a package, formation of an insulating layer, (2) hermetic sealing of a plasma display-panel, an insulating layer and a dielectric. Examples include formation of a body layer, formation of a barrier rib, and (3) sealing of a magnetic head-core or between a core and a slider. Moreover, the form at the time of use does not have a restriction | limiting in particular, What is necessary is just to shape | mold and use it in various forms according to the use, such as powder form, plate shape, rod shape.
[0020]
【Example】
Hereinafter, the bismuth-based low-melting glass composition of the present invention will be described in detail based on examples.
[0021]
Tables 1 and 2 show examples of the present invention (sample Nos. 2, 5, and 10 ). Other samples are reference examples.
[0022]
[Table 1]
Figure 0003814810
[0023]
[Table 2]
Figure 0003814810
[0024]
Each sample in the table was prepared as follows.
[0025]
First, a glass batch prepared by mixing various oxides, carbonates and the like so as to have the glass composition shown in the table was prepared, put in a platinum crucible and melted at 900 to 1100 ° C. for 2 hours, and then the molten glass was made of stainless steel. The mold was poured into the mold. About each obtained sample, the glass transition point, the thermal expansion coefficient in 30-300 degreeC, a calcination temperature, and crystalline or non-crystalline were evaluated. The results are shown in the table.
[0026]
As is apparent from the table, each sample of the examples has a glass transition point of 390 to 452 ° C. and a thermal expansion coefficient of 90 to 110 × 10 −7 / ° C. in a temperature range of 30 to 300 ° C., and a firing temperature. It was 600 ° C. or lower. Sample No. 2 is non-crystalline. 5 and no . 10 was crystalline.
[0027]
The transition point was determined by a differential thermal analyzer (DTA). The thermal expansion coefficient was measured using a push rod type thermal expansion coefficient measuring device after polishing the molded glass body into a cylindrical shape having a diameter of 4 mm and a length of 40 mm. The firing temperature was determined as follows. First, the glass body was pulverized to obtain a glass powder, and a glass powder having a weight corresponding to the true specific gravity of the glass was press-molded into a button shape having an outer diameter of 20 mm and a height of about 5 mm using a mold. Next, this button was placed on a plate glass, placed in an electric furnace, heated at a rate of 10 ° C./min, and held at various temperatures for 10 minutes. The temperature at which the outer diameter of the button thus obtained was in the range of 21 to 22 mm was defined as the firing temperature. The crystallinity or non-crystallinity was determined by observing the appearance of the sample after being heated at the firing temperature for 10 minutes with a microscope and evaluating from the crystal precipitation state.
[0028]
【The invention's effect】
As described above, since the bismuth-based glass composition of the present invention does not contain PbO, there is no concern of causing environmental problems. Moreover, since it can bake at the temperature of 650 degrees C or less, it can be used for uses, such as adhesion | attachment of an electronic component, sealing, and coating | cover, as an alternative material of the low melting glass containing conventional PbO.

Claims (1)

重量百分率でＢｉ2Ｏ3 ２０〜８０％、Ｂ2Ｏ3 ５〜３５％、ＢａＯ ０〜３５％、ＳｒＯ ０〜３０％、ＢａＯ＋ＳｒＯ ５〜４０％（ただし５％を含まず）、ＺｎＯ ０〜９％、ＣａＯ ０〜１０％、Ｆｅ2Ｏ3 ０〜５％、ＣｕＯ ２〜１０％、ＺｎＯ＋ＣａＯ＋Ｆｅ2Ｏ3＋ＣｕＯ ２〜２０％、ＳｉＯ2 ０〜８％、Ａｌ2Ｏ3 ０〜５％、Ｃｓ2Ｏ ０〜５％、Ｆ2 ０〜５％の組成を有し、本質的にＰｂＯを含有しないことを特徴とするビスマス系ガラス組成物。Bi 2 O 3 20-80% by weight percentage, B 2 O 3 5-35%, BaO 0-35%, SrO 0-30%, BaO + SrO 5-40% (but not including 5%) , ZnO 0 9%, CaO 0~10%, Fe 2 O 3 0~5%, CuO 2 ~10%, ZnO + CaO + Fe 2 O 3 + CuO 2 ~20%, SiO 2 0~8%, Al 2 O 3 0~5%, cs 2 O 0 to 5%, F 2 has a 0-5% composition, essentially bismuth-based glass composition characterized by containing no PbO.
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