JPS5945620B2 - Low melting point sealing composition - Google Patents
Low melting point sealing compositionInfo
- Publication number
- JPS5945620B2 JPS5945620B2 JP12634378A JP12634378A JPS5945620B2 JP S5945620 B2 JPS5945620 B2 JP S5945620B2 JP 12634378 A JP12634378 A JP 12634378A JP 12634378 A JP12634378 A JP 12634378A JP S5945620 B2 JPS5945620 B2 JP S5945620B2
- Authority
- JP
- Japan
- Prior art keywords
- melting point
- low melting
- powder
- sealing
- sealing composition
- 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.)
- Expired
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
- 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
- C03C8/245—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 containing more than 50% lead oxide, by weight
Description
【発明の詳細な説明】
本発明は、低融点封着用組成物、特に４５０℃以下の封
着温度で、アルミナを使用した１、Ｃ、パッケージを封
着できる低融点封着用組成物に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a low melting point sealing composition, particularly a low melting point sealing composition that can seal 1, C, packages using alumina at a sealing temperature of 450° C. or lower. be.
Ｉ−Ｃ・パッケージに用いられている封着用組成物には
、熱失透性のものと非晶質のものとがある。There are two types of sealing compositions used in IC packages: thermally devitrified compositions and amorphous compositions.
熱失透性の封着用組成物は封着温度が高く、封着時間が
長いので熱経済的に不利であるばかりでなく、製造工程
のインデックスからも好ましくない。そこで、封着温度
が低く、封着時間の短い非晶質の低融点ガラスを主体と
する封着用組成物が用いられているが、熱衝撃強度、耐
酸性などに問題があつた。本出願人はこれらの欠点を改
善し、熱衝撃強度、耐酸性に優れた非晶質の封着用組成
物を開発し、既に特許出願した（特公昭５３一２９１６
２）。これは、低融点ガラス粉末に、チタン酸鉛粉末と
珪酸ジルコニウム粉末とを添加したものである。ところ
が、最近、珪酸ジルコニウム中の不純物に微量の放射性
物質が含まれており、これから放射されるα線が集積度
の高いＩ−Ｃ・素子のソフトエラーを引き起すというこ
とが伝えられている。A thermally devitrified sealing composition has a high sealing temperature and a long sealing time, so it is not only disadvantageous thermoeconomically but also unfavorable from the viewpoint of manufacturing process index. Therefore, sealing compositions mainly composed of amorphous low-melting glass that have a low sealing temperature and a short sealing time have been used, but they have had problems with thermal shock strength, acid resistance, and the like. The present applicant has improved these drawbacks and developed an amorphous sealing composition with excellent thermal shock strength and acid resistance, and has already filed a patent application (Japanese Patent Publication No. 53-12916).
2). This is made by adding lead titanate powder and zirconium silicate powder to a low melting point glass powder. However, it has recently been reported that impurities in zirconium silicate contain trace amounts of radioactive substances, and that the alpha rays emitted from the impurities cause soft errors in highly integrated IC devices.
本発明は、低い温度で短時間に封着でき、熱衝撃強度及
び耐酸性に優れ、且つ放射性物質を含まない新規な封着
用組成物を提供するものである。本発明の封着用組成物
は、屈伏点が３５０℃以下の非晶質の鉛、硼酸系低融点
ガラス粉末とウイレマイト（Ｚｎ２Ｓｉ０４）粉末とチ
タン酸鉛（ＰｂＯ、ＴｉＯ２）粉末とから成り、これら
の割合が重量比で低融点ガラス粉末４５〜７０％、ウイ
レマイト粉末１〜３５％、チタン酸鉛粉末１〜５０％、
ウイレマイト粉末とチタン酸鉛粉末の含量３０〜３５％
の範囲にあり、前記非晶質の鉛、硼酸系低融点ガラス粉
末を重量％でＰｂ０７０〜９０）Ｂ２０３１０〜１５、
５ｉ０２０．５〜５、Ｚｎ００〜５、Ａ１２０３０〜５
、ＰｂＦ２０〜１５としたことを特徴とする。低融点ガ
ラス、ウイレマイト、チタン酸鉛の混合割合を上記のよ
うに限定したのは、次の理由による。The present invention provides a novel sealing composition that can be sealed at low temperatures in a short time, has excellent thermal shock strength and acid resistance, and does not contain radioactive substances. The sealing composition of the present invention is composed of amorphous lead having a yield point of 350°C or less, boric acid-based low melting point glass powder, willemite (Zn2Si04) powder, and lead titanate (PbO, TiO2) powder. The weight ratio is low melting point glass powder 45-70%, willemite powder 1-35%, lead titanate powder 1-50%,
Willemite powder and lead titanate powder content 30-35%
Pb070-90) B20310-15,
5i020.5~5, Zn00~5, A12030~5
, PbF20-15. The reason why the mixing ratio of low melting point glass, willemite, and lead titanate is limited as described above is as follows.
低融点ガラスが４５％に満たない場合は、封着用組成物
の流動性が悪く良好な封着が得られず、７０％を超える
と熱膨張係数が大きくなり過ぎて、熱衝撃強度が小さく
なる。ウイレマイトが３５％を超える場合、及びチタン
酸鉛が５０％を超える場合は共に流動性が悪くなり良好
な封着が得られず、ウイレマイトとチタン酸鉛の含量が
３０％に満たない場合は熱膨張係数が大きくなり過ぎて
熱衝撃強度が小さくなり、」方５５％を超える場合は流
動性が悪くなり、良好な封着が得られない。さらに低融
点ガラス粉末の組成を限定した理由は、以下に示す通り
である。If the low melting point glass content is less than 45%, the sealing composition has poor fluidity and good sealing cannot be obtained, and if it exceeds 70%, the thermal expansion coefficient becomes too large and the thermal shock strength decreases. . If the content of willemite exceeds 35% and if the content of lead titanate exceeds 50%, the fluidity will deteriorate and good sealing will not be obtained.If the content of willemite and lead titanate is less than 30%, heat If the expansion coefficient becomes too large, the thermal shock strength becomes small, and if it exceeds 55%, the fluidity becomes poor and good sealing cannot be obtained. Furthermore, the reason why the composition of the low melting point glass powder was limited is as follows.
ＰｂＯが７０％のときは封着温度が高くなり、９０％以
上のときはガラス化が困難になる。When PbO is 70%, the sealing temperature becomes high, and when it is 90% or more, vitrification becomes difficult.
Ｂ２Ｏ３が１０％以下のときは封着時に好ましくない失
透化を呈し、１５％以上のときは封着温度が高くなる。
ＳｉＯ２が０．５％以下のときは耐酸性が悪くなり、５
％以上ではガラスの粘度が高くなつて封着組成物の流動
性が悪くなり良好な封着が得られない。Ａｌ２Ｏ３、Ｚ
ｎＯを加えると耐酸性が向上するが、ＺｎＯが５％以上
になると封着時に失透化し、Ａｌ２Ｏ３が５％以上にな
るとガラスの粘度が高くなり封着組成物の流動性が悪く
なつて良好な封着が得られない。ＰｂＦ２を加えると屈
伏点が下がるが、１５％以上になると封着時に失透化す
る。以下に本発明の実施例について説明する。When B2O3 is 10% or less, undesirable devitrification occurs during sealing, and when it is 15% or more, the sealing temperature becomes high.
When SiO2 is less than 0.5%, acid resistance deteriorates, and 5
% or more, the viscosity of the glass becomes high and the fluidity of the sealing composition deteriorates, making it impossible to obtain good sealing. Al2O3,Z
Adding nO improves acid resistance, but when ZnO exceeds 5%, devitrification occurs during sealing, and when Al2O3 exceeds 5%, the viscosity of the glass increases and the fluidity of the sealing composition deteriorates, making it unfavorable. A good seal cannot be obtained. Addition of PbF2 lowers the yield point, but if it exceeds 15%, devitrification occurs during sealing. Examples of the present invention will be described below.
非晶質の鉛、硼酸系低融点ガラスの実施例を第１表に示
す。Examples of amorphous lead and boric acid-based low melting point glasses are shown in Table 1.
本発明の低融点封着用組成物の実施例を第２表に示す。Examples of the low melting point sealing composition of the present invention are shown in Table 2.
第１表に示した低融点ガラスは、光明丹、硼酸、石粉及
び水酸化アルミニウム又は、亜鉛華、弗化鉛を第１表に
示す組成になるように調合し、白金るつぼに入れて約９
００℃で３０分間溶融した後、板状に成形し、アルミナ
ボールミルで粉砕し、１５０メツシユのステンレス篩で
分級した。The low melting point glass shown in Table 1 is prepared by mixing Komyotan, boric acid, stone powder, and aluminum hydroxide, zinc white, and lead fluoride to the composition shown in Table 1, and placing it in a platinum crucible for about 90 minutes.
After melting at 00° C. for 30 minutes, it was formed into a plate shape, pulverized with an alumina ball mill, and classified with a 150 mesh stainless steel sieve.
ウイレマイトは、ＺｎＯとＳｉＯ２のモル比が２：１と
なるように亜鉛華及び光学石粉を調合し、１４５０℃で
１５時間焼成した後アルミナボールミルで粉砕し、３２
５メツシユのステンレス篩で分級した。チタゾ酸鉛は、
ＴｉＯ２とＰｂＯのモル比が１：１になるように、酸化
チタン及びりサージを調合し、１１５０℃で２時間焼成
した後、アルミナボールミルで粉砕し、３２５メツシユ
のステンレス篩で分級した。Willemite is produced by mixing zinc white and optical stone powder so that the molar ratio of ZnO and SiO2 is 2:1, firing it at 1450°C for 15 hours, and then crushing it with an alumina ball mill.
It was classified using a 5-mesh stainless steel sieve. Lead titazate is
Titanium oxide and trisurge were prepared so that the molar ratio of TiO2 and PbO was 1:1, fired at 1150° C. for 2 hours, ground in an alumina ball mill, and classified with a 325 mesh stainless steel sieve.
上記のようにして得た低融点ガラス粉末、ウイレマイト
粉末、チタン酸鉛粉末を第２表に示す割合に混合し、通
常行なわれているようにビークルを添加してペーストを
作成し、アルミナセラミツクに印刷して封着した。The low melting point glass powder, willemite powder, and lead titanate powder obtained as described above were mixed in the proportions shown in Table 2, a vehicle was added as usual to create a paste, and alumina ceramic was mixed. Printed and sealed.
得られたＩ−Ｃ・バツケージは、熱衝撃強度、耐酸性に
優れた良好な封着状態を示した。この封着物を観察した
ところ、非晶質のガラス中にウイレマイトがその粒状の
形態をとどめて混在していることが認められた。The obtained I-C package showed a good sealing state with excellent thermal shock strength and acid resistance. When this sealed product was observed, it was found that willemite remained in its granular form and was mixed in the amorphous glass.
Claims (1)
融点ガラス粉末とウイレマイト粉末とチタン酸鉛粉末と
から成り、これらの割合が重量比で、▲数式、化学式、
表等があります▼の範囲にあり、前記非晶質の鉛、硼酸
系低融点ガラス粉末を、重量％で、ＰｂＯ７０〜９０、
Ｂ＿２Ｏ＿３１０〜１５、ＳｉＯ＿２０．５〜５、Ｚｎ
Ｏ０〜５、Ａｌ＿２Ｏ＿３０〜５、ＰｂＦ＿２０〜１５
とした低融点封着用組成物。1 Consists of amorphous lead with a yield point of 350°C or less, boric acid-based low melting point glass powder, willemite powder, and lead titanate powder, the proportions of which are expressed in weight ratio, ▲ mathematical formula, chemical formula,
There are tables, etc. in the range ▼, and the above amorphous lead, boric acid-based low melting point glass powder, in weight%, PbO70-90,
B_2O_310-15, SiO_20.5-5, Zn
O0~5, Al_2O_30~5, PbF_20~15
A low melting point sealing composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12634378A JPS5945620B2 (en) | 1978-10-13 | 1978-10-13 | Low melting point sealing composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12634378A JPS5945620B2 (en) | 1978-10-13 | 1978-10-13 | Low melting point sealing composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5551736A JPS5551736A (en) | 1980-04-15 |
| JPS5945620B2 true JPS5945620B2 (en) | 1984-11-07 |
Family
ID=14932806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12634378A Expired JPS5945620B2 (en) | 1978-10-13 | 1978-10-13 | Low melting point sealing composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5945620B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01170393A (en) * | 1987-12-21 | 1989-07-05 | Matsushita Electric Ind Co Ltd | Electric cleaner |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63149710U (en) * | 1987-03-25 | 1988-10-03 | ||
| JPH0822763B2 (en) * | 1989-03-01 | 1996-03-06 | 日本電気硝子株式会社 | Low melting point sealing composition |
| DE4106796A1 (en) * | 1991-03-04 | 1991-11-07 | Wollnik Hermann | A FLIGHT-TIME MASS SPECTROMETER AS SECOND LEVEL OF AN MS-MS SYSTEM |
-
1978
- 1978-10-13 JP JP12634378A patent/JPS5945620B2/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01170393A (en) * | 1987-12-21 | 1989-07-05 | Matsushita Electric Ind Co Ltd | Electric cleaner |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5551736A (en) | 1980-04-15 |
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