JPH05170481A - Seal bonding composition having low melting point - Google Patents
Seal bonding composition having low melting pointInfo
- Publication number
- JPH05170481A JPH05170481A JP35597491A JP35597491A JPH05170481A JP H05170481 A JPH05170481 A JP H05170481A JP 35597491 A JP35597491 A JP 35597491A JP 35597491 A JP35597491 A JP 35597491A JP H05170481 A JPH05170481 A JP H05170481A
- Authority
- JP
- Japan
- Prior art keywords
- melting point
- glass
- powder
- low melting
- low
- 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.)
- Pending
Links
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
- C03C3/12—Silica-free oxide glass compositions
- C03C3/122—Silica-free oxide glass compositions containing oxides of As, Sb, Bi, Mo, W, V, Te as glass formers
-
- 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
- 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
Landscapes
- 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
Description
【０００１】[0001]
【産業上の利用分野】本発明は、低融点封着組成物に関
し、より具体的には、半導体集積回路、水晶振動子等の
熱に弱い素子を搭載したセラミックパッケージや金属パ
ッケージを気密封着するのに好適な低融点封着組成物に
関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a low melting point sealing composition, and more specifically, to a hermetically sealing ceramic package or metal package having a heat-sensitive element such as a semiconductor integrated circuit or a crystal unit mounted thereon. The present invention relates to a low melting point sealing composition suitable for
【０００２】[0002]
【従来の技術】従来より半導体集積回路や水晶振動子等
の素子を搭載した高信頼性のパッケージの気密封着に
は、ガラス粉末を用いた低融点封着組成物が使用されて
いる。2. Description of the Related Art Conventionally, a low melting point sealing composition using glass powder has been used for hermetically sealing a highly reliable package on which elements such as a semiconductor integrated circuit and a crystal oscillator are mounted.
【０００３】このような低融点封着組成物としては、Ｐ
ｂＯ−Ｂ2 Ｏ3 系ガラスに、チタン酸鉛やウイレマイト
等の低膨張の耐火性物質粉末を添加したものが広く知ら
れている。しかしながらこの系のガラスを用いた低融点
封着組成物は、４００℃以下の温度で封着することが困
難であるため、集積度の高いＬＳＩや特殊な水晶振動子
等の熱に極めて敏感な素子を搭載したパッケージの気密
封着を行う場合には、素子の特性が劣化する恐れがあ
る。As such a low melting point sealing composition, P
to bO-B 2 O 3 based glass, a material obtained by adding refractory material powder of a low expansion, such as lead titanate or willemite is widely known. However, since a low melting point sealing composition using this type of glass is difficult to seal at a temperature of 400 ° C. or less, it is extremely sensitive to heat such as highly integrated LSI and special crystal oscillators. When airtight sealing of a package having an element mounted thereon is performed, the characteristics of the element may be deteriorated.
【０００４】近年、上記事情から、より低い温度で封着
することが可能な低融点封着組成物が各種提案されてい
る。例えば、特開昭６３−３１５５３６号公報には、Ｐ
ｂＯ−Ｂ2 Ｏ3 −Ｔｌ2 Ｏ系ガラスを使用した低融点封
着組成物が示され、また特表昭６３−５０２５８３号公
報には、ＰｂＯ−Ｖ2 Ｏ5 −Ｂｉ2 Ｏ3 系ガラスを使用
した低融点封着組成物が示され、これらの低融点封着組
成物は、使用するガラスの転移点が低く、４００℃以下
での封着が可能であるが、いずれも問題を有している。In view of the above circumstances, various low-melting point sealing compositions capable of sealing at lower temperatures have been proposed in recent years. For example, in JP-A-63-315536, P
bO-B 2 O 3 -Tl low melting point sealing composition using 2 O-based glass is shown, also in the Kohyo Sho 63-502583 JP, PbO-V 2 O 5 -Bi 2 O 3 based glass A low-melting point sealing composition using is shown. These low-melting point sealing compositions have a low transition point of the glass used and can be sealed at 400 ° C. or lower, but all have problems. is doing.
【０００５】[0005]
【発明が解決しようとする課題】すなわち特開昭６３−
３１５５３６号公報に開示の封着組成物は、３５０℃で
封着することが可能であるが、毒性の強いＴｌ2 Ｏを多
量に含有するため、製造時や封着作業時に粉塵の飛散を
防ぐ設備が必要であり、実用上の問題がある。SUMMARY OF THE INVENTION That is, JP-A-63-
The sealing composition disclosed in Japanese Patent No. 315536 can be sealed at 350 ° C., but contains a large amount of highly toxic Tl 2 O, and thus prevents scattering of dust during manufacturing or sealing work. Equipment is required and there are practical problems.
【０００６】また特表昭６３−５０２５８３号公報に開
示の封着組成物は、封着温度を３３０〜３７０℃程度ま
で低下させることが可能であるが、結晶化傾向が強く、
加熱すると結晶が析出して流動性が悪くなるため、低温
で封着するには、封着時に金属クリップ等によって相当
の荷重をかけなければならない。The sealing composition disclosed in Japanese Patent Publication No. 63-502583 can reduce the sealing temperature to about 330 to 370 ° C., but has a strong tendency to crystallize.
When heated, crystals precipitate and the flowability deteriorates. Therefore, in order to perform sealing at a low temperature, a considerable load must be applied with a metal clip or the like during sealing.
【０００７】本発明の目的は、Ｔｌ等の有害物質を含有
せず、しかも荷重をかけることなく、３３０〜３５０℃
の低温でパッケージを気密封着することが可能な低融点
封着組成物を提供することである。The object of the present invention is to contain no harmful substances such as Tl, and without applying a load, at 330 to 350 ° C.
To provide a low melting point sealing composition capable of hermetically sealing a package at low temperature.
【０００８】[0008]
【課題を解決するための手段】本発明者は、上記目的を
達成すべく、数々の研究を重ねた結果、ＴｅＯ2 −Ｖ2
Ｏ5 −ＰｂＯ−Ａｇ2 Ｏ系ガラスのガラス転移点が非常
に低く、しかも結晶化傾向が少なく、この系のガラスの
各構成成分を所定の割合で含有させることによって、３
５０℃以下の封着温度を有する低融点封着組成物を得る
ことが可能であることを見いだし、本発明として提案す
るものである。Means for Solving the Problems The present inventor has conducted a number of studies in order to achieve the above object, and as a result, TeO 2 --V 2
The glass transition point of O 5 -PbO-Ag 2 O based glass is very low, and the crystallization tendency is low. By incorporating each constituent component of the glass of this system in a predetermined ratio, 3
It was found that it is possible to obtain a low melting point sealing composition having a sealing temperature of 50 ° C. or lower, and it is proposed as the present invention.
【０００９】すなわち本発明の低融点封着組成物は、重
量百分率で、ＴｅＯ2 １５〜３４％、Ｖ2 Ｏ5 １５
〜４５％、ＰｂＯ ５〜３５％、Ａｇ2 Ｏ ５〜４０％
の組成を有するガラス粉末からなることを特徴とする。That is, the low melting point sealing composition of the present invention has a weight percentage of TeO 2 of 15 to 34% and V 2 O 5 of 15.
~45%, PbO 5~35%, Ag 2 O 5~40%
It is characterized by comprising glass powder having the composition of.
【００１０】また本発明の他の態様の低融点封着組成物
は、上記ガラス粉末４５〜９０体積％と、耐火性物質粉
末１０〜５５体積％からなることを特徴とする。A low melting point sealing composition according to another aspect of the present invention is characterized by comprising 45 to 90% by volume of the above glass powder and 10 to 55% by volume of a refractory substance powder.
【００１１】[0011]
【作用】本発明の低融点封着組成物において、ガラス粉
末の組成を上記のように限定した理由は、以下のとおり
である。The reason for limiting the composition of the glass powder in the low melting point sealing composition of the present invention as described above is as follows.
【００１２】ＴｅＯ2 は、本発明のガラスの骨格を形成
する成分であり、その含有量は、１５〜３４％である。
１５％より少ない場合は、ガラスが失透しやすいため、
安定なガラスが得られない。一方、３４％より多い場合
は、ガラスの熱膨張係数が著しく大きくなり、熱膨張係
数を低くするために低膨張性の耐火性物質粉末を添加し
た場合、ガラス粉末と耐火性物質粉末との熱膨張係数の
差に起因して微小クラックが発生しやすくなる。TeO 2 is a component forming the skeleton of the glass of the present invention, and its content is 15 to 34%.
If it is less than 15%, the glass tends to devitrify,
Stable glass cannot be obtained. On the other hand, when the content is more than 34%, the coefficient of thermal expansion of the glass becomes remarkably large. Microcracks are likely to occur due to the difference in expansion coefficient.
【００１３】Ｖ2 Ｏ5 も、本発明のガラスの骨格を形成
する成分であり、その含有量は、１５〜４５％である。
この含有範囲をはずれる場合は、ガラスの結晶化傾向が
著しくなり、良好な封着ができなくなる。V 2 O 5 is also a component forming the skeleton of the glass of the present invention, and its content is 15 to 45%.
If the content is out of this range, the crystallization tendency of glass becomes remarkable, and good sealing cannot be achieved.
【００１４】ＰｂＯは、ガラスを低融点化する成分であ
り、その含有量は、５〜３５％である。５％より少ない
場合は、封着時にガラスが結晶化を起こして流動し難く
なり、結晶化傾向が大きくなる。一方、３５％より多い
場合は、ガラスの粘度が高くなって、十分に流動しな
い。PbO is a component that lowers the melting point of glass, and its content is 5 to 35%. If it is less than 5%, the glass will be crystallized during sealing and it will be difficult for it to flow, and the crystallization tendency will be large. On the other hand, when it is more than 35%, the viscosity of the glass becomes high and the glass does not flow sufficiently.
【００１５】Ａｇ2 Ｏも、ガラスを低融点化する成分で
あり、その含有量は、５〜４０％である。５％より少な
い場合は、ガラスの粘度が高くなって、十分に流動しな
い。一方、４０％より多い場合は、ガラスの熱膨張係数
が高くなりすぎる。Ag 2 O is also a component that lowers the melting point of glass, and its content is 5 to 40%. When it is less than 5%, the viscosity of the glass becomes high and the glass does not flow sufficiently. On the other hand, when it is more than 40%, the thermal expansion coefficient of the glass becomes too high.
【００１６】尚、本発明においては、特性を損なわない
範囲で、上記成分以外にも、ＺｎＯ、Ｂｉ2 Ｏ3 、Ｃｕ
2 Ｏ、Ａｌ2 Ｏ3 、ＳｉＯ2 、Ｂ2 Ｏ3 、ＷＯ3 、Ｍｏ
Ｏ3、Ｎｂ2 Ｏ5 、ＳｒＯ、ＢａＯ、Ｃｓ2 Ｏの１者あ
るいは２者以上を選択して、１０％まで含有させること
が可能である。In the present invention, in addition to the above components, ZnO, Bi 2 O 3 and Cu may be used as long as the characteristics are not impaired.
2 O, Al 2 O 3 , SiO 2 , B 2 O 3 , WO 3 , Mo
One or two or more of O 3 , Nb 2 O 5 , SrO, BaO, and Cs 2 O can be selected and contained up to 10%.
【００１７】また本発明においては、上記ガラス粉末に
耐火性物質粉末を混合することによって、熱膨張係数を
調節したり、機械的強度を向上させることができる。Further, in the present invention, by mixing the glass powder with the refractory substance powder, the coefficient of thermal expansion can be adjusted and the mechanical strength can be improved.
【００１８】この場合、ガラス粉末４５〜９０体積％
と、耐火性物質粉末１０〜５５体積％からなるように混
合するが、各粉末の混合割合をこのように限定した理由
は、以下のとおりである。In this case, 45 to 90% by volume of glass powder
The refractory substance powder is mixed so as to be 10 to 55% by volume. The reason for limiting the mixing ratio of each powder in this way is as follows.
【００１９】すなわち耐火性物質粉末が１０体積％より
も少ない場合は、低融点封着組成物の熱膨張係数を調整
したり、機械的強度を向上させるという効果が小さく、
また５５体積％より多い場合は、低融点封着組成物の流
動性が著しく低下して気密性の高い封着が行えなくな
る。That is, when the refractory substance powder is less than 10% by volume, the effect of adjusting the thermal expansion coefficient of the low melting point sealing composition and improving the mechanical strength is small,
On the other hand, if it is more than 55% by volume, the fluidity of the low-melting point sealing composition is remarkably reduced, and highly airtight sealing cannot be performed.
【００２０】本発明の低融点封着組成物の熱膨張係数
を、ＩＣパッケージとして使用されるアルミナパッケー
ジの熱膨張係数に合致させるためには、特に熱膨張係数
の低い耐火性物質粉末を添加する必要がある。この種の
耐火性物質粉末としては、本出願人の出願に係る特願昭
６１−８７５４２号、特願平１−８６９５８号及び特願
平３−１９７１３６号に示すチタン酸鉛固溶体粉末が有
用であり、さらに通常のジルコン粉末、酸化すず粉末、
酸化ニオブ粉末、チタン酸鉛粉末、β−ユークリプタイ
ト粉末、コージェライト粉末等を併用することも可能で
ある。In order to match the coefficient of thermal expansion of the low melting point sealing composition of the present invention with the coefficient of thermal expansion of an alumina package used as an IC package, a refractory substance powder having a particularly low coefficient of thermal expansion is added. There is a need. As this type of refractory substance powder, the lead titanate solid solution powders shown in Japanese Patent Application Nos. 61-87542, 1-86958 and 3-197136, which are filed by the applicant, are useful. Yes, normal zircon powder, tin oxide powder,
It is also possible to use niobium oxide powder, lead titanate powder, β-eucryptite powder, cordierite powder and the like together.
【００２１】また本発明の低融点封着組成物をアルミナ
パッケージに比べて高い熱膨張係数を有する金属パッケ
ージに使用する場合、ガラス粉末に添加される耐火性物
質粉末には、特に熱膨張係数が低いことは要求されな
い。そのためこの場合は、通常のアルミナ粉末、ジルコ
ニア粉末、チタニア粉末、スピネル粉末、すず酸亜鉛粉
末等を使用することができる。When the low melting point sealing composition of the present invention is used in a metal package having a higher coefficient of thermal expansion than that of an alumina package, the refractory material powder added to the glass powder has a particularly high coefficient of thermal expansion. Low is not required. Therefore, in this case, usual alumina powder, zirconia powder, titania powder, spinel powder, zinc stannate powder, etc. can be used.
【００２２】[0022]
【実施例】以下、本発明の低融点封着組成物を実施例に
基づいて詳細に説明する。EXAMPLES The low melting point sealing composition of the present invention will be described in detail below with reference to examples.
【００２３】表１は、本発明において使用するガラス粉
末を示すものである。Table 1 shows the glass powder used in the present invention.
【００２４】[0024]
【表１】 [Table 1]
【００２５】表１のガラス粉末（試料Ａ〜Ｉ）は、以下
のように調製した。The glass powders in Table 1 (Samples A to I) were prepared as follows.
【００２６】まず表１の組成になるように二酸化テル
ル、五酸化バナジウム、鉛丹、酸化銀、亜鉛華、酸化ビ
スマス、酸化第二銅、五酸化ニオブ、アルミナ、三酸化
タングステン、酸化セリウムを調合し、混合した。次い
でこれを白金ルツボに入れ、電気炉で７００℃、１時間
の条件で溶融し、薄板状に成形した後、ボールミルで粉
砕し、２５０メッシュ（目開き６３μｍ）の篩を通過さ
せた。First, tellurium dioxide, vanadium pentoxide, red lead, silver oxide, zinc oxide, bismuth oxide, cupric oxide, niobium pentoxide, alumina, tungsten trioxide, and cerium oxide are prepared so as to have the composition shown in Table 1. And mixed. Then, this was placed in a platinum crucible, melted in an electric furnace at 700 ° C. for 1 hour, molded into a thin plate, crushed with a ball mill, and passed through a 250 mesh (mesh opening 63 μm) sieve.
【００２７】表１から明らかなように、いずれのガラス
粉末も転移点が２１０〜２２０℃と極めて低く、また結
晶は析出しておらず、良好な流動性を有していた。As is clear from Table 1, all the glass powders had a very low transition point of 210 to 220 ° C., and no crystals were precipitated, and they had good fluidity.
【００２８】尚、流動性の判断は、ガラスの比重に相当
する重量の粉末試料を外径２０ｍｍ、高さ約５ｍｍのボ
タンに成形した後、３５０℃、１０分間の条件で加熱
し、このときのボタンの直径が２３ｍｍを超えるものを
良とした。また結晶析出の有無は、流動性試験後のボタ
ン表面を顕微鏡で観察し、結晶が全く認められなかった
ものを良とした。The fluidity is determined by molding a powder sample having a weight equivalent to the specific gravity of glass into a button having an outer diameter of 20 mm and a height of about 5 mm, and then heating at 350 ° C. for 10 minutes. A button having a diameter of more than 23 mm was considered good. Regarding the presence or absence of crystal precipitation, the button surface after the fluidity test was observed under a microscope and no crystal was observed at all, which was regarded as good.
【００２９】また表２は、表１のガラス粉末Ｂ及びＤに
各種の耐火性物質粉末を混合した低膨張封着組成物の実
施例（試料Ｎｏ．１〜７）を示すものである。Table 2 shows examples (Sample Nos. 1 to 7) of low expansion sealing compositions in which the glass powders B and D of Table 1 are mixed with various refractory substance powders.
【００３０】[0030]
【表２】 [Table 2]
【００３１】表２から明らかなように、Ｎｏ．１〜５の
試料は、アルミナセラミックの熱膨張係数（７０×１０
-7／℃）に近い熱膨張係数を有し、またＮｏ．６と７の
試料は、アルミニウム−シリコン合金の熱膨張係数（１
６０×１０-7／℃）に近い熱膨張係数を有していた。As is clear from Table 2, No. Samples 1 to 5 are thermal expansion coefficients of alumina ceramics (70 × 10
No. 7 / ° C.) and a thermal expansion coefficient close to that of No. The samples of 6 and 7 have a coefficient of thermal expansion (1
It had a coefficient of thermal expansion close to 60 × 10 −7 / ° C.).
【００３２】また各試料を、通常行われているようにビ
ークルを添加してペースト状にした後、Ｎｏ．１〜５の
試料をアルミナセラミック基板に印刷し、Ｎｏ．６と７
の試料をアルミニウム−シリコン合金基板に印刷し、封
着温度を測定したところ、いずれも３３０〜３４０℃の
低温で、荷重をかけることなく封着が可能であった。Further, each sample was made into a paste by adding a vehicle as usual, and then No. The samples Nos. 1 to 5 were printed on an alumina ceramic substrate and No. 6 and 7
The sample was printed on an aluminum-silicon alloy substrate and the sealing temperature was measured. As a result, it was possible to seal at a low temperature of 330 to 340 ° C. without applying a load.
【００３３】表２で使用した各耐火性物質粉末は、以下
のようにして作製したものである。The refractory substance powders used in Table 2 are produced as follows.
【００３４】Ｐｂ0.75Ｃａ0.25ＴｉＯ2 は、リサージ、
炭酸カルシウム、酸化チタンを重量百分率で、ＰｂＯ６
４％、ＣａＯ５％、ＴｉＯ2 ３１％になるように調合
し、乾式混合した後、１１７０℃で５時間焼成し、次い
で粉砕して３５０メッシュ（目開き４５μｍ）の篩を通
過させた。Pb 0.75 Ca 0.25 TiO 2 is a litharge,
Calcium carbonate and titanium oxide in PbO6 by weight percentage
4%, CaO 5%, and TiO 2 31% were mixed, dry-mixed, calcined at 1170 ° C. for 5 hours, and then pulverized and passed through a 350-mesh sieve (opening 45 μm).
【００３５】Ｐｂ0.90Ｃａ0.10Ｆｅ0.15Ｎｂ0.15Ｔｉ
0.70Ｏ3 は、リサージ、酸化チタン、酸化第二鉄、五酸
化ニオブ、炭酸カルシウムを重量百分率で、ＰｂＯ６
８．２％、ＣａＯ １．９％、Ｆｅ2 Ｏ3 ４．１％、
Ｎｂ2 Ｏ5 ６．８％、ＴｉＯ2 １９．０％になるよう
に調合し、乾式混合した後、１２５０℃で５時間焼成
し、次いで粉砕して３５０メッシュ（目開き４５μｍ）
の篩を通過させた。Pb 0.90 Ca 0.10 Fe 0.15 Nb 0.15 Ti
0.70 O 3 is litharge, titanium oxide, ferric oxide, niobium pentoxide, calcium carbonate in a weight percentage, PbO 6
8.2%, CaO 1.9%, Fe 2 O 3 4.1%,
Nb 2 O 5 6.8% and TiO 2 19.0% were blended, dry-mixed, baked at 1250 ° C. for 5 hours, and then pulverized to 350 mesh (opening 45 μm).
Through the sieve.
【００３６】ＳｎＯ2 は、酸化第二錫と、焼結助剤とし
ての亜鉛華を、重量百分率で、ＳｎＯ2 ９９％、ＺｎＯ
１％になるように調合、乾式混合し、１４８０℃で１６
時間焼成後、粉砕し、３５０メッシュの篩を通過させ
た。SnO 2 is composed of stannic oxide and zinc white as a sintering aid in a weight percentage of 99% SnO 2 and ZnO 2.
Formulated to 1%, dry-mixed, 16 at 1480 ° C
After firing for an hour, it was crushed and passed through a 350 mesh screen.
【００３７】Ｎｂ2 Ｏ5 は、五酸化ニオブ試薬を１３５
０℃で５時間焼成した後、粉砕し、次いで３５０メッシ
ュの篩を通過させた。Nb 2 O 5 is a niobium pentoxide reagent 135
After firing at 0 ° C. for 5 hours, it was ground and then passed through a 350 mesh screen.
【００３８】ＳｉＺｒＯ4 は、天然のジルコンサンドを
一旦ソーダ分解し、塩酸に溶解した後、濃縮結晶化を繰
り返すことによって、α線放出物質であるＵ、Ｔｈの極
めて少ないオキシ塩化ジルコニウムにし、アルカリ中和
後、加熱して精製ＺｒＯ2 を得た。次にこの精製したＺ
ｒＯ2 に高純度珪石粉、酸化第二鉄を重量比でＺｒＯ2
６６％、ＳｉＯ2 ３２％、Ｆｅ2 Ｏ3 ２％の組成になる
ように調合し、混合した後、１４００℃で１６時間焼成
し、次いでこの焼成物を粉砕し、２５０メッシュのステ
ンレス篩を通過させた。SiZrO 4 is obtained by once decomposing natural zircon sand with soda, dissolving it in hydrochloric acid, and repeating concentrated crystallization to obtain zirconium oxychloride, which is an α-ray-emitting substance having extremely small amounts of U and Th, and is used in an alkali. After the addition, the mixture was heated to obtain purified ZrO 2 . Then this purified Z
High-purity silica stone powder and ferric oxide were added to rO 2 in a weight ratio of ZrO 2
The composition was 66%, SiO 2 32%, Fe 2 O 3 2%, and after mixing, it was fired at 1400 ° C. for 16 hours, then the fired product was crushed and passed through a 250 mesh stainless sieve. Let
【００３９】Ａｌ2 Ｏ3 は、電融アルミナを粉砕し、３
５０メッシュのステンレス篩を通過させた。Al 2 O 3 is prepared by pulverizing fused alumina to obtain 3
It was passed through a 50 mesh stainless sieve.
【００４０】２ＺｎＯ・ＳｎＯ2 は、亜鉛華と酸化すず
を重量百分率で、ＺｎＯ５１．９％、ＳｎＯ2 ４８．１
％になるように調合、乾式混合し、１４５０℃で１６時
間焼成した後、粉砕し、次いで３５０メッシュのステン
レス篩を通過させた。2ZnO.SnO 2 is zinc oxide 51.9%, SnO 2 48.1 in terms of weight percentage of zinc white and tin oxide.
%, Mixed by dry mixing, baked at 1450 ° C. for 16 hours, pulverized, and then passed through a 350-mesh stainless sieve.
【００４１】尚、各表における転移点と熱膨張係数は、
ディラトメーターによって測定された熱膨張曲線から求
めた。The transition point and the coefficient of thermal expansion in each table are
It was determined from the thermal expansion curve measured by a dilatometer.
【００４２】[0042]
【発明の効果】以上のように本発明の低融点封着組成物
は、有害物質を含有せず、しかも荷重をかけることな
く、３５０℃以下の低温でパッケージを気密封着するこ
とが可能であるため、特にＬＳＩや特殊な水晶振動子等
の熱に極めて弱い素子を搭載したセラミックパッケージ
や金属パッケージを気密封着するのに好適である。INDUSTRIAL APPLICABILITY As described above, the low melting point sealing composition of the present invention can be hermetically sealed at a low temperature of 350 ° C. or lower without containing a harmful substance and without applying a load. Therefore, it is particularly suitable for hermetically sealing a ceramic package or a metal package on which an extremely weak element such as an LSI or a special crystal oscillator is mounted.
Claims (2)
％、Ｖ2 Ｏ5 １５〜４５％、ＰｂＯ ５〜３５％、Ａ
ｇ2 Ｏ ５〜４０％の組成を有するガラス粉末からなる
ことを特徴とする低融点封着組成物。1. TeO 2 15-34 by weight percentage.
%, V 2 O 5 15 to 45%, PbO 5 to 35%, A
A low melting point sealing composition comprising a glass powder having a composition of g 2 O 5 to 40%.
％、Ｖ2 Ｏ5 １５〜４５％、ＰｂＯ ５〜３５％、Ａ
ｇ2 Ｏ ５〜４０％の組成を有するガラス粉末４５〜９
０体積％と、耐火性物質粉末１０〜５５体積％からなる
ことを特徴とする低融点封着組成物。2. TeO 2 15-34 by weight percentage.
%, V 2 O 5 15 to 45%, PbO 5 to 35%, A
glass powder 45-9 with g 2 O 5 to 40% of the composition
A low melting point sealing composition comprising 0% by volume and a refractory substance powder of 10 to 55% by volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35597491A JPH05170481A (en) | 1991-12-20 | 1991-12-20 | Seal bonding composition having low melting point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35597491A JPH05170481A (en) | 1991-12-20 | 1991-12-20 | Seal bonding composition having low melting point |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05170481A true JPH05170481A (en) | 1993-07-09 |
Family
ID=18446684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35597491A Pending JPH05170481A (en) | 1991-12-20 | 1991-12-20 | Seal bonding composition having low melting point |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05170481A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014156369A (en) * | 2013-02-15 | 2014-08-28 | Hitachi Ltd | Glass and manufacturing method thereof |
| CN104039547A (en) * | 2011-12-26 | 2014-09-10 | 株式会社日立制作所 | Laminate, and organic el element, window and solar cell module, each using same |
| JP2015163587A (en) * | 2015-04-23 | 2015-09-10 | 旭硝子株式会社 | Lead-free glass for sealing, sealing material and sealing material paste |
| US20150279700A1 (en) * | 2012-11-09 | 2015-10-01 | Hitachi, Ltd. | Bonded Structure and Production Method Therefor |
| JP2016050136A (en) * | 2014-08-29 | 2016-04-11 | 日立化成株式会社 | Lead-free low-melting point glass composition and low-temperature sealing glass frit, low-temperature sealing glass paste, conductive material and conductive glass paste containing the same, and glass-sealed component and electric and electronic component using them |
| JP2019052054A (en) * | 2017-09-14 | 2019-04-04 | Ｄｏｗａエレクトロニクス株式会社 | Silver coated tin tellurium glass powder, manufacturing method therefor, and conductive paste |
| WO2024057823A1 (en) * | 2022-09-14 | 2024-03-21 | 日本電気硝子株式会社 | Sealant-layer-equipped glass substrate and method for producing hermetic package |
-
1991
- 1991-12-20 JP JP35597491A patent/JPH05170481A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104039547A (en) * | 2011-12-26 | 2014-09-10 | 株式会社日立制作所 | Laminate, and organic el element, window and solar cell module, each using same |
| CN104039547B (en) * | 2011-12-26 | 2015-11-25 | 株式会社日立制作所 | Duplexer and use its organic EL element, window, solar module |
| US20150279700A1 (en) * | 2012-11-09 | 2015-10-01 | Hitachi, Ltd. | Bonded Structure and Production Method Therefor |
| US9824900B2 (en) * | 2012-11-09 | 2017-11-21 | Hitachi, Ltd. | Bonded structure and production method therefor |
| JP2014156369A (en) * | 2013-02-15 | 2014-08-28 | Hitachi Ltd | Glass and manufacturing method thereof |
| JP2016050136A (en) * | 2014-08-29 | 2016-04-11 | 日立化成株式会社 | Lead-free low-melting point glass composition and low-temperature sealing glass frit, low-temperature sealing glass paste, conductive material and conductive glass paste containing the same, and glass-sealed component and electric and electronic component using them |
| JP2015163587A (en) * | 2015-04-23 | 2015-09-10 | 旭硝子株式会社 | Lead-free glass for sealing, sealing material and sealing material paste |
| JP2019052054A (en) * | 2017-09-14 | 2019-04-04 | Ｄｏｗａエレクトロニクス株式会社 | Silver coated tin tellurium glass powder, manufacturing method therefor, and conductive paste |
| WO2024057823A1 (en) * | 2022-09-14 | 2024-03-21 | 日本電気硝子株式会社 | Sealant-layer-equipped glass substrate and method for producing hermetic package |
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