JPS6236040A - Low-melting point sealing glass - Google Patents
Low-melting point sealing glassInfo
- Publication number
- JPS6236040A JPS6236040A JP17327185A JP17327185A JPS6236040A JP S6236040 A JPS6236040 A JP S6236040A JP 17327185 A JP17327185 A JP 17327185A JP 17327185 A JP17327185 A JP 17327185A JP S6236040 A JPS6236040 A JP S6236040A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- pbo
- zno
- sealing
- 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.)
- Withdrawn
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
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
【発明の詳細な説明】
［産業上の利用分野］
本発明は、低融点でかつ耐水性に優れた封着用硝子に関
するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a sealing glass having a low melting point and excellent water resistance.
［従来の技術］
従来より、低融（４００〜８００℃程度）での封着には
ＰｂＯ−Ｂ’ｚ ０３−９ Ｉ０２系もしくはＰｂＯ−
８２０＋ −２１１０系が広く用いられてきた。これら
の系は低融点で封着できるが、耐水性が悪く、封着面の
研磨や水処理により、封着面が容易に浸食されてしまう
問題があった。[Prior art] Conventionally, PbO-B'z 03-9 I02 series or PbO-
The 820+-2110 series has been widely used. Although these systems have a low melting point and can be sealed, they have poor water resistance and have the problem that the sealing surface is easily eroded by polishing or water treatment.
例えば、硝子・セラミックスによる半導体パッケージの
封着に用いると、封着模本に浸漬することにより表面に
白い反応生成物が生成する。また、磁気ヘッドのギャッ
プ形成、接合に用いた場合、木による研磨で封着面が浸
食される。For example, when used to seal semiconductor packages made of glass or ceramics, a white reaction product is generated on the surface by immersing the sealing model. Furthermore, when used for gap formation or bonding of magnetic heads, the sealing surface is eroded by polishing with wood.
［発明の解決しようとする問題点］
本発明の目的は、低融（４００〜６００℃程度）で封着
でき、かつ耐水性に優れた封着用の硝子・で、特に磁気
ヘッドの接合用に好適に用いられる封着用硝子を提供す
ることである。[Problems to be Solved by the Invention] An object of the present invention is to provide a sealing glass that can be sealed at a low melting point (approximately 400 to 600°C) and has excellent water resistance, and is particularly suitable for bonding magnetic heads. An object of the present invention is to provide a sealing glass that can be suitably used.
［問題点を解決するための手段］
末完ＩＪＩの目的はモル％表示で木質的にＴｅＯ２ｌＯ
〜８０
ＰｂＯ ８〜５０８２０
３ ３〜４０Ｚｎ０
３〜３０ＴｅＯｚ＋ＰｂＯ＋
Ｂ２Ｏ１＋ＺｎＯ＞ ７５Ｗ（ｈ ＋ＭＯ０３０〜２５
Ｓ ｉ０７ ＋５ｎ０２ ＋Ｔ ｉ０２ ”ＺｒＯ２０
〜１０Ａ１２０ｘ＋Ｌａ２Ｏ３０” １０
Ｍｇ０＋ＣａＯ＋ＳｒＯ＋Ｂａ０ ０〜
２５からなる低融点封着用硝子を提供する。[Means to solve the problem] The purpose of Shukan IJI is to express TeO2lO in terms of mol%.
~80 PbO 8~50820
3 3～40Zn0
3~30TeOz+PbO+
B2O1+ZnO> 75W (h +MO030~25 S i07 +5n02 +T i02 ”ZrO20
~10A120x+La2O30" 10 Mg0+CaO+SrO+Ba0 0~
To provide a low melting point sealing glass consisting of No. 25.
次に本発明の組成限定理由について説明する。Next, the reason for limiting the composition of the present invention will be explained.
ＴｅＯ２が１０％より少ないと硝子の耐水性が失われる
。 ＴｅＯ２が８０％を越えると、硝子の失透性が強く
安定した封着ができない、 ｐｂｏが８％より少ないと
硝子の粘性が大きくなり、低温で封着できなくなる。
ｐｂｏが５０％を越えると、硝子の失透性が強く安定し
た封着ができない。If TeO2 is less than 10%, the water resistance of the glass will be lost. If TeO2 exceeds 80%, the devitrification of the glass is strong and stable sealing cannot be achieved. If pbo is less than 8%, the viscosity of the glass increases, making it impossible to seal at low temperatures.
If pbo exceeds 50%, the devitrification of the glass is so strong that stable sealing cannot be achieved.
Ｂ２Ｏ３が３％より少ないと、硝子の失透性が強く安定
した封着ができない、またＢ２Ｏ３が４０％を越えると
、耐水性が劣化してくる。 ＺｎＯが３％より少ないと
硝子の耐水性が劣化する。 ＺｎＯが２５％を越えると
硝子の失透性が強くなり過ぎ、封着が不０■能になる。When the B2O3 content is less than 3%, the devitrification of the glass is so strong that stable sealing cannot be achieved, and when the B2O3 content exceeds 40%, the water resistance deteriorates. If ZnO is less than 3%, the water resistance of the glass will deteriorate. If the ZnO content exceeds 25%, the devitrification of the glass becomes too strong, making sealing impossible.
ＴｅＯ２，ＰｂＯ、Ｂ２Ｏ３、ＺｎＯの総￥が７５％
以Ｆでは耐水性が悪くなるので好ましくない。The total amount of TeO2, PbO, B2O3, and ZnO is 75%
F or less is not preferable because the water resistance deteriorates.
ＷＣｈ 、ＭｎＯ２はＴｅＯ２系硝子の膨張係数を下げ
るが、総量で２５％を越えると硝子が失透し易くなり好
ましくない、 ５ｉ０２．ＴｉＯ２，ＺｒＯ２は硝子の
膨張係数を下げ耐水性を向上させ、更に硝子をより安定
にする効果があるが、総量で１０％を越えると均質な硝
子が得られ難く、未熔解物が残存し易くなり好ましくな
い、＾１２０３．Ｌａ２Ｏ３は５ｎ０２ 。WCh and MnO2 lower the expansion coefficient of TeO2-based glass, but if the total amount exceeds 25%, the glass tends to devitrify, which is undesirable. 5i02. TiO2 and ZrO2 have the effect of lowering the expansion coefficient of glass, improving water resistance, and making glass more stable, but if the total amount exceeds 10%, it is difficult to obtain homogeneous glass, and unmelted substances tend to remain. I don't like it, ^1203. La2O3 is 5n02.
ＴｉＯ２，ＺｒＯ＋ と同様な働きをするが、総量で１
０％を越えると未熔解物として残存し、均質な硝子が得
られ難くなり好ましくない、 ＭｇＯ，Ｃ：ａｏ、Ｓｒ
Ｏ。It works in the same way as TiO2 and ZrO+, but the total amount is 1
If it exceeds 0%, it remains unmelted and makes it difficult to obtain homogeneous glass, which is undesirable. MgO, C:ao, Sr
O.
ＢａＯは硝子の粘性を調整する作用があるが、総量で２
５％を越えると硝子が失透性となり好ましくない。BaO has the effect of adjusting the viscosity of glass, but the total amount is 2
If it exceeds 5%, the glass becomes devitrified, which is not preferable.
より好ましい範囲は上記範囲中、
Ｔｌ！０２ ２０〜７０％、ＰｂＯ１Ｑ〜４０％、８
２０３５ 〜３５％、 Ｚｎ０ ５〜２５％、 丁
ｅ０７＋ＰｂＯ＋Ｂ２Ｏ３＋ ＺｎＯ＞８０゜ＷＯ３
＋Ｎｏ０３ ０〜２０％、 Ｓｎ０？＋Ｔ ｉ０２ ＋
ＺｎＯ２０〜７ ％。Among the above ranges, a more preferable range is Tl! 02 20-70%, PbO1Q-40%, 8
2035 ~35%, Zn0 5~25%, Dinge07+PbO+B2O3+ ZnO>80°WO3
+No03 0-20%, Sn0? +T i02 +
ZnO 20-7%.
Ａｌ２Ｏ＊＋Ｌａ２Ｏ３０〜７ ％、 １ｌｌＨＯ
＋ＣａＯ＋ＳｒＯ＋ＢａＯＱ 〜２０％である０以上の
成分の外に）ｌｎＯ２，Ｃｏｏ、Ｎｉｐ。Al2O*+La2O30~7%, 1llHO
+CaO+SrO+BaOQ ~20% in addition to 0 or more components) lnO2, Coo, Nip.
Ｆｅ２Ｏ３等の着色剤、５ｂ２０３ 、 ＡＳ２０３等
の清澄剤を各１モル％まで添加できる。Coloring agents such as Fe2O3 and clarifying agents such as 5b203 and AS203 can be added up to 1 mol% each.
本発明、による硝子は例えば次の様にして製造される。Glass according to the present invention is manufactured, for example, in the following manner.
酸化物からなる原料を目標組成となる様に調合した後８
００〜１２５０℃の範囲で加熱して、０．３〜２時間保
持し硝子化する０次いで、溶融硝子を水砕するか、水冷
ロールによって粗砕する０次いで、この粗砕硝子をボー
ルミル等により更に粉砕し、平均径で２〜１０μ−程度
の粒度とする。かくして得られた硝子により封着するに
は例えば次の様な方法がある。After mixing raw materials consisting of oxides to the target composition 8
Heat in the range of 00 to 1250°C and hold for 0.3 to 2 hours to form vitrification.Next, the molten glass is crushed into water or coarsely crushed with a water-cooled roll.Next, the crushed glass is crushed by a ball mill or the like. It is further pulverized to have a particle size of about 2 to 10 microns in average diameter. There are, for example, the following methods for sealing with the glass thus obtained.
硝子粉末をニトロセルロースを １〜３ ｗｔ％含むブ
チルカルピトールアセテート溶液（有機ビヒクル）と混
合し、扱い安い粘度に調整する。The glass powder is mixed with a butylcarpitol acetate solution (organic vehicle) containing 1-3 wt% nitrocellulose and adjusted to a manageable viscosity.
次いで、これを被接着面に塗布した後、封着部を硝子の
作業温度まで加熱し、５〜１５分間保持することによっ
て封着が行なわれる。Next, after applying this to the surface to be bonded, the sealing portion is heated to the working temperature of glass and held for 5 to 15 minutes to effect sealing.
［実施例］
表１に示した組成となる様に各酸化物原料を調合し、ア
ルミナ乳ばちで混合しバッチ５０ｇを調整した０次いで
これを白金坩堝に入れ、１０００℃に加熱し３０分間保
持することにより硝子化した。更に、これをよく磨いた
鉄板上に流し出し１表１に記載した硝子転移点（Ｔｇ）
より５℃程度高い温度より徐冷し各種特性を調べるため
の硝子試料を製造した。[Example] Each oxide raw material was prepared to have the composition shown in Table 1, and mixed in an alumina mortar to prepare a batch of 50 g.Then, this was placed in a platinum crucible and heated to 1000°C for 30 minutes. It became vitrified by holding it. Furthermore, pour this onto a well-polished iron plate and obtain the glass transition point (Tg) listed in Table 1.
Glass samples were manufactured by slowly cooling the glass from a temperature approximately 5°C higher than the original temperature to examine various properties.
この硝子について同表の記載の特性を調べた。各特性に
ついては次の様に測定したものである。The properties listed in the same table were investigated for this glass. Each characteristic was measured as follows.
Ｔｇ及びＳｐＣ軟化点）はそれぞれ示差熱分析計に最初
の吸熱ピークと次の吸熱ピークの開始点である。Tg and SpC softening point) are the starting points of the first and second endothermic peaks in the differential thermal analyzer, respectively.
作業温度は硝子をスライスカー／ トし約０．２ｍｍの
厚みとし、これを膨張係数が１１０〜目０！１０− ’
／℃の間にあるソーダ舎カリΦライム系の板硝子基板の
間に海人し、加熱後封着できた温度である。膨張係数は
２０１１１１！５φのサンプルを研磨して作製し、示差
膨張形にてΔ一定した３０〜３００℃間の値である。耐
水性は流し出した硝子を約ｌＯ■角１厘■厚に切断し表
面を酸化セリウムで鏡面に仕上げた後、佛騰水で１０分
間煮沸した後の表面の変化状態で、Ａは表面の変質が認
められなかったもの、日は表面に曇りが生じたもの、Ｃ
は表面が白濁したものである。The working temperature is to slice the glass to a thickness of about 0.2 mm, and set the expansion coefficient to 110 to 0!10-'.
/°C is the temperature at which it was possible to seal between the Soda Potash Φ Lime plate glass substrates after heating. The expansion coefficient was prepared by polishing a sample of 201111!5φ, and was a value between 30 and 300° C. with a constant Δ in the differential expansion type. Water resistance is the change in the surface after cutting the poured glass into pieces approximately 10cm square and 1cm thick, finishing the surface with cerium oxide to a mirror finish, and then boiling it in Buddha water for 10 minutes.A is the change in the surface. No alteration was observed, the surface was cloudy on the day, C
The surface is cloudy.
陥、１３は比較例で、従来のＰｂＯ−８＋０３−５ｉＯ
；＋−ＺｎＯ系の硝子である。同表より明らかなように
従来の硝子では、煮沸水中で１０分間煮沸すると、白濁
してしまうが、本発明の硝子（Ｎｏ、１−１２）は白濁
する事はなく耐水性に優れている事がわかる。また作業
温度も６００℃以下で十分に低い温度で使用することが
できる。13 is a comparative example, which is a conventional PbO-8+03-5iO
;+-ZnO glass. As is clear from the table, conventional glass becomes cloudy when boiled in boiling water for 10 minutes, but the glass of the present invention (No. 1-12) does not become cloudy and has excellent water resistance. I understand. Further, the working temperature is 600° C. or lower, which is a sufficiently low temperature.
［発１１の効果］
本発明の硝子は耐水性に優れており、硝子月１Ｅ後の水
を使用した研磨や高温高湿での使用に十分耐えることが
できる。この特性は特に磁気ヘッド用硝子材料や車載用
電子部品に要求されており、これらの用途に好適に用い
ることができる。[Effects of Efficiency 11] The glass of the present invention has excellent water resistance and can sufficiently withstand polishing using water after glass month 1E and use at high temperature and high humidity. This property is particularly required for glass materials for magnetic heads and electronic components for vehicles, and can be suitably used for these applications.
Claims (1)
０〜８０ ＰｂＯ
８〜５０ Ｂ＿２Ｏ＿３
３〜４０ ＺｎＯ
３〜３０ ＴｅＯ＿２＋ＰｂＯ＋Ｂ＿２Ｏ＿３＋ＺｎＯ
＞７５ ＷＯ＿３＋ＭｏＯ＿３
０〜２５ ＳｉＯ＿２＋ＳｎＯ＿２＋ＴｉＯ＿２＋ＺｒＯ＿２
０〜１０ Ａｌ＿２Ｏ＿３＋Ｌａ＿２Ｏ＿３
０〜１０ ＭｇＯ＋ＣａＯ＋ＳｒＯ＋ＢａＯ
０〜２５ からなる低融点封着用硝子。(1) Essentially TeO_2 1 in mol%
0-80 PbO
8～50 B_2O_3
3-40 ZnO
3~30 TeO_2+PbO+B_2O_3+ZnO
>75 WO_3+MoO_3
0~25 SiO_2+SnO_2+TiO_2+ZrO_2
0~10 Al_2O_3+La_2O_3
0~10 MgO+CaO+SrO+BaO
Low melting point sealing glass consisting of 0 to 25.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17327185A JPS6236040A (en) | 1985-08-08 | 1985-08-08 | Low-melting point sealing glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17327185A JPS6236040A (en) | 1985-08-08 | 1985-08-08 | Low-melting point sealing glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6236040A true JPS6236040A (en) | 1987-02-17 |
Family
ID=15957353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17327185A Withdrawn JPS6236040A (en) | 1985-08-08 | 1985-08-08 | Low-melting point sealing glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6236040A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252547A (en) * | 1988-03-31 | 1989-10-09 | Sharp Corp | Low-temperature-fusible glass composition |
| JPH01308844A (en) * | 1988-06-07 | 1989-12-13 | Sharp Corp | Low-temperature fusible glass composition |
| WO1992000925A1 (en) * | 1990-07-09 | 1992-01-23 | Cookson Group Plc | Glass compositions |
| US5245492A (en) * | 1989-11-28 | 1993-09-14 | Matsushita Electric Industrial Co., Ltd. | Magnetic head |
| US5273948A (en) * | 1991-06-24 | 1993-12-28 | Hitachi Metals, Ltd. | Bonding glass for assembling a magnetic head, and a magnetic head |
| US5283212A (en) * | 1990-11-28 | 1994-02-01 | Corning Incorporated | Thallium germanate, tellurite, and antimonite glasses |
| JPH06290410A (en) * | 1993-03-31 | 1994-10-18 | Sony Corp | Magnetic head |
| JP2013533187A (en) * | 2010-05-04 | 2013-08-22 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Thick film pastes containing lead-tellurium-lithium-titanium-oxides and their use in the manufacture of semiconductor devices |
| US20140175340A1 (en) * | 2012-12-21 | 2014-06-26 | Young Wook Choi | Glass frit, composition for solar cell electrodes including the same, and electrode fabricated using the same |
| US10658528B2 (en) | 2017-04-18 | 2020-05-19 | Dupont Electronics, Inc. | Conductive paste composition and semiconductor devices made therewith |
-
1985
- 1985-08-08 JP JP17327185A patent/JPS6236040A/en not_active Withdrawn
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252547A (en) * | 1988-03-31 | 1989-10-09 | Sharp Corp | Low-temperature-fusible glass composition |
| JPH01308844A (en) * | 1988-06-07 | 1989-12-13 | Sharp Corp | Low-temperature fusible glass composition |
| US5245492A (en) * | 1989-11-28 | 1993-09-14 | Matsushita Electric Industrial Co., Ltd. | Magnetic head |
| WO1992000925A1 (en) * | 1990-07-09 | 1992-01-23 | Cookson Group Plc | Glass compositions |
| WO1992000924A1 (en) * | 1990-07-09 | 1992-01-23 | Cookson Group Plc | Tellurite glass compositions |
| US5283212A (en) * | 1990-11-28 | 1994-02-01 | Corning Incorporated | Thallium germanate, tellurite, and antimonite glasses |
| US5283211A (en) * | 1990-11-28 | 1994-02-01 | Corning Incorporated | Thallium germanate, tellurite, and antimonite glasses |
| US5273948A (en) * | 1991-06-24 | 1993-12-28 | Hitachi Metals, Ltd. | Bonding glass for assembling a magnetic head, and a magnetic head |
| JPH06290410A (en) * | 1993-03-31 | 1994-10-18 | Sony Corp | Magnetic head |
| US9722100B2 (en) | 2010-05-04 | 2017-08-01 | E I Du Pont De Nemours And Company | Thick-film pastes containing lead-tellurium-lithium-oxides, and their use in the manufacture of semiconductor devices |
| US8889979B2 (en) | 2010-05-04 | 2014-11-18 | E I Du Pont De Nemours And Company | Thick-film pastes containing lead—tellurium—lithium—titanium—oxides, and their use in the manufacture of semiconductor devices |
| US8889980B2 (en) | 2010-05-04 | 2014-11-18 | E I Du Pont De Nemours And Company | Thick-film pastes containing lead—tellurium—lithium—oxides, and their use in the manufacture of semiconductor devices |
| US8895843B2 (en) | 2010-05-04 | 2014-11-25 | E I Du Pont De Nemours And Company | Thick-film pastes containing lead-tellurium-boron-oxides, and their use in the manufacture of semiconductor devices |
| JP2013533187A (en) * | 2010-05-04 | 2013-08-22 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Thick film pastes containing lead-tellurium-lithium-titanium-oxides and their use in the manufacture of semiconductor devices |
| US10069020B2 (en) | 2010-05-04 | 2018-09-04 | E I Du Pont De Nemours And Company | Thick-film pastes containing lead- and tellurium-oxides, and their use in the manufacture of semiconductor devices |
| US10468542B2 (en) | 2010-05-04 | 2019-11-05 | Dupont Electronics, Inc. | Thick-film pastes containing lead-tellurium-lithium-oxides, and their use in the manufacture of semiconductor devices |
| US10559703B2 (en) | 2010-05-04 | 2020-02-11 | Dupont Electronics, Inc. | Thick-film pastes containing lead-tellurium-boron-oxides, and their use in the manufacture of semiconductor devices |
| US11043605B2 (en) | 2010-05-04 | 2021-06-22 | E I Du Pont De Nemours And Company | Thick-film pastes containing lead- and tellurium-oxides, and their use in the manufacture of semiconductor devices |
| US20140175340A1 (en) * | 2012-12-21 | 2014-06-26 | Young Wook Choi | Glass frit, composition for solar cell electrodes including the same, and electrode fabricated using the same |
| US9512032B2 (en) * | 2012-12-21 | 2016-12-06 | Cheil Industries, Inc. | Glass frit, composition for solar cell electrodes including the same, and electrode fabricated using the same |
| US10658528B2 (en) | 2017-04-18 | 2020-05-19 | Dupont Electronics, Inc. | Conductive paste composition and semiconductor devices made therewith |
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