JP2987039B2 - Glass for bonding and sealing - Google Patents
Glass for bonding and sealingInfo
- Publication number
- JP2987039B2 JP2987039B2 JP5271453A JP27145393A JP2987039B2 JP 2987039 B2 JP2987039 B2 JP 2987039B2 JP 5271453 A JP5271453 A JP 5271453A JP 27145393 A JP27145393 A JP 27145393A JP 2987039 B2 JP2987039 B2 JP 2987039B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- sealing
- pbo
- bonding
- water resistance
- 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 - Fee Related
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
- C03C3/16—Silica-free oxide glass compositions 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
- 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
Description
【０００１】[0001]
【産業上の利用分野】本発明は接着・封止用ガラスにか
かり、特に磁気ヘッドの封着に好適な接着・封止用ガラ
スに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a glass for bonding and sealing, and more particularly to a glass for bonding and sealing suitable for sealing a magnetic head.
【０００２】[0002]
【従来技術とその問題点】接着・封止用ガラスとしてPb
O 系、特に PbO−B2O3系、 PbO−B2O3−SiO2系、PbO −
B2O3−ZnO 系、 PbO−B2O3−SiO2−Al2O3 系等の低融点
ガラスが広く採用されることはよく知られるところであ
る。[Prior art and its problems] Pb as glass for bonding and sealing
O system, in particular PbO-B 2 O 3 -based, PbO-B 2 O 3 -SiO 2 system, PbO -
It is well known that low melting point glass such as B 2 O 3 —ZnO system or PbO—B 2 O 3 —SiO 2 —Al 2 O 3 system is widely used.
【０００３】しかし上記低融点ガラスは、金属、セラミ
ックの接着・封止用としては勿論、磁気ヘッド封着用と
しては耐水、耐薬品性が不充分で、被接着材料とも反応
し被接着材料を変質し易い、ガラスの硬度が低い等の難
点があり、またPbO を多量に含有するため、加熱加工作
業中に有害なPbO の揮散により作業環境を悪化させ、あ
るいは水と接触するとPbイオンが溶出し公害問題を誘起
する等、問題点も多い。However, the above-mentioned low-melting glass has insufficient water resistance and chemical resistance not only for bonding and sealing of metals and ceramics but also for sealing a magnetic head, and reacts with a material to be bonded to deteriorate the material to be bonded. It has drawbacks such as easy processing, low glass hardness, and contains a large amount of PbO, which worsens the working environment due to harmful PbO volatilization during heating processing, or Pb ions are eluted when it comes into contact with water. There are many problems such as inducing pollution problems.
【０００４】これに対し、特開昭61−36135 号、特開昭
61−111935号には、V2O5−P2O5系にTeO2等を含み、磁気
ヘッドの接着・封止用に供する低融点ガラスが開示され
ている。しかし耐水・耐薬品性や硬度等に難点があり、
またV2O5自体熱安定性に劣り、着色不透明になり易い等
の問題もある。On the other hand, Japanese Patent Application Laid-Open No. 61-36135 and
No. 61-111935 discloses a low-melting glass that contains TeO 2 or the like in a V 2 O 5 —P 2 O 5 system and is used for bonding and sealing a magnetic head. However, there are difficulties in water resistance, chemical resistance, hardness, etc.
In addition, V 2 O 5 itself is inferior in thermal stability and tends to be colored and opaque.
【０００５】他方、特開昭62−128946号にはTeO2−P2O5
−PbO −(ZnO＋Li2O) 系に各種任意成分を含み、光学材
料として好適で低融点ガラスでもあるテルライトガラス
が開示されている。しかし磁気ヘッド封着用ガラスとし
ての開示、示唆はしてない。またPbO が多いケースにお
いては前記同様の公害上の問題が危惧される。さらに、
開示実施例は耐水・耐薬品性に劣っていたり、硬度が不
充分であったりする等、磁気ヘッドの接着・封止用とし
ては満足できるものではない。On the other hand, Japanese Patent Application Laid-Open No. Sho 62-128946 discloses that TeO 2 -P 2 O 5
Tellurite glass, which contains various optional components in a —PbO— (ZnO + Li 2 O) system and is suitable as an optical material and is also a low-melting glass, is disclosed. However, it does not disclose or suggest glass for sealing a magnetic head. Also, in the case of a large amount of PbO, there is a concern about the same pollution problem as described above. further,
The disclosed examples are not satisfactory for adhesion and sealing of a magnetic head, such as poor water and chemical resistance and insufficient hardness.
【０００６】なお磁気ヘッドの接着・封止用ガラスにお
いては、熱膨張率が磁性体のそれとよく適合しているこ
と、作業温度が磁性体の特性を損ねない程度の温度域で
あること、耐水、耐薬品性に優れること、高い硬度を有
すること、機械的強度が高いこと、透視性を有するこ
と、磁性体との相互反応がないこと、磁気的絶縁性に優
れること等が要求される。これらファクターは二律背反
的な要素もあっていずれをも十二分に満足させるのは困
難であるが、本発明は多くのファクターにおいて適合
し、あるいは公知のガラスに比べ優れた接着・封止用ガ
ラスを提供するものである。The glass for bonding and sealing the magnetic head must have a coefficient of thermal expansion that is well compatible with that of the magnetic material, a working temperature in a temperature range that does not impair the characteristics of the magnetic material, and a water resistance. It is required to be excellent in chemical resistance, high in hardness, high in mechanical strength, transparent, have no interaction with a magnetic substance, and excellent in magnetic insulation. These factors are inconsistent with each other, and it is difficult to satisfy all of them.However, the present invention is suitable for many factors, or is superior in adhesion and sealing glass compared to known glass. Is provided.
【０００７】[0007]
【問題点を解決するための手段】本発明は、 mol％表示
で、P2O5 20 〜60％、TeO2 10 〜50％、PbO 0 〜＜１
％、ZnO 0 〜20％、BaO 0 〜20％、Li2O 0〜20％、Bi2O
3 0 〜10％の範囲で、PbO、ZnO 、BaO 、Li2OおよびBi2
O3 の和が25〜40％である接着・封止用ガラスである。[Means for Solving the Problems] The present invention provides the following
And PTwoOFive 20-60%, TeOTwo 10-50%, PbO0 to <1
%, ZnO 0-20%, BaO 0-20%, LiTwoO 0-20%, BiTwoO
Three In the range of 0-10%, PbO, ZnO, BaO, LiTwoO and BiTwo
OThree For bonding and sealing with a sum of 25 to 40%Is.
【０００８】なお、特に磁気ヘッドの接着・封止用ガラ
スにおいては、熱膨張率が磁性体の100 〜140 ／℃程度
の熱膨張率とよく適合していること、作業温度が磁性体
の特性を損ねない 500〜 600℃程度であること、耐水、
耐薬品性に優れること、比較的高い硬度を有すること、
機械的強度が高いこと、透視性を有すること、磁性体と
の相互反応がないこと、磁気的絶縁性に優れること等が
要求されるが、本発明の接着・封止用ガラスは多くのフ
ァクターにおいて適合し、あるいは公知のガラスに比べ
優れた特性を示すものである。Particularly, in the glass for bonding and sealing the magnetic head, the coefficient of thermal expansion is well matched to the coefficient of thermal expansion of the magnetic material of about 100 to 140 / ° C. 500-600 ℃, water resistance,
Excellent in chemical resistance, having relatively high hardness,
High mechanical strength, high transparency, no interaction with magnetic materials, excellent magnetic insulation, etc. are required, but the bonding and sealing glass of the present invention has many factors. Or exhibit superior properties as compared with known glasses.
【０００９】本成分系において、P2O5は mol％で20〜60
％の範囲においてガラス形成が良好で安定しており、他
方60％を越えるとガラスの耐水、耐薬品性を悪化させ、
また20％未満であるとガラス形成を不安定にする。TeO2
は同様に10〜50％の範囲においてガラス形成が良好で安
定しており、50％を越えるとガラス形成を不安定にし、
ガラスの硬度を低下させ、10％未満ではガラスの耐水性
を悪化させる等不具合が生ずる。In this component system, P 2 O 5 is 20 to 60 mol%.
%, The glass formation is good and stable, while if it exceeds 60%, the water resistance and chemical resistance of the glass deteriorate,
If it is less than 20%, glass formation becomes unstable. TeO 2
Is similarly good and stable in the range of 10 to 50%, and if it exceeds 50%, the glass formation becomes unstable,
If the hardness of the glass is lowered, and if it is less than 10%, problems such as deterioration of the water resistance of the glass occur.
【００１０】PbO は安定した低融点ガラスを得るうえで
きわめて有用であるが、ガラスの硬度を低下させ、水へ
の溶出による公害問題も大きいので1％未満とする。[0010] PbO is extremely useful for obtaining a stable low-melting glass. However, PbO reduces the hardness of the glass and causes a large pollution problem due to elution into water.
【００１１】BaO はPbO の前記欠点を補ううえで重要で
あり、特にPbO を含有しないケースにおいては 5％以上
の導入が好ましい。なお、20％を越えると耐失透性が悪
化する。[0011] BaO is important in compensating the above-mentioned disadvantages of PbO, and particularly when PbO is not contained, it is preferable to introduce 5% or more. If it exceeds 20%, the devitrification resistance deteriorates.
【００１２】Li2Oは溶融性を改善し安定したガラスを
得、ガラスの耐水性を向上するうえで有効であるが、20
％を越えると耐水性を悪化させ、接着に際して被接着体
との反応も起生し易いので20％以下とする。なお 5〜20
％の範囲で導入することが望ましい。Li 2 O is effective in improving the melting property to obtain a stable glass and improving the water resistance of the glass.
%, The water resistance is degraded, and a reaction with the adherend is likely to occur during bonding. 5-20
% Is desirably introduced.
【００１３】ZnO もガラスの安定性、耐水性向上に有効
であるが、20％を越えると失透が生じ易く、ガラス形成
も困難となる。Bi2O3 はガラスの耐水性、硬度向上に有
効であるが、10％を越えるとガラス形成を不安定とし、
ガラスを製造する際の溶融・成形性に劣る。[0013] ZnO is also effective for improving the stability and water resistance of the glass. However, if it exceeds 20%, devitrification tends to occur and glass formation becomes difficult. Bi 2 O 3 is effective in improving the water resistance and hardness of glass, but if it exceeds 10%, glass formation becomes unstable,
Poor melting / molding properties when producing glass.
【００１４】さらに、PbO 、ZnO 、BaO 、Li2OおよびBi
2O3 の和が40％を越えると、相対的にガラス形成成分で
あるP2O5およびTiO2が過少となりガラス形成が困難とな
り、他方25％未満ではガラスの耐水性、硬度、あるいは
ガラス製造時の均質性、清澄性を含めた易溶性において
劣る。Further, PbO, ZnO, BaO, Li 2 O and Bi
If the sum of 2 O 3 exceeds 40%, the glass forming components P 2 O 5 and TiO 2 become relatively small, making glass formation difficult, while if less than 25%, the water resistance, hardness, or Poor in solubility, including homogeneity and clarity during production.
【００１５】なお、硬度、耐水性等を向上するために例
えばSiO2、TiO2、Al2O3 、SrO 等をガラスの安定性を向
上するためにB2O3を、溶融性の改善のためにNa2O、K2O
、MgO 、CaO 等を、あるいは熱膨張率を調整するため
に前掲した成分を 5％以下程度の範囲で適宜導入するこ
とができる。[0015] Incidentally, the hardness, the B 2 O 3 in order to improve the water resistance and the like such as SiO 2, TiO 2, Al 2 O 3, SrO or the like to improve the stability of the glass, the improvement of meltability For Na 2 O, K 2 O
, MgO, CaO, etc., or the above-mentioned components for adjusting the coefficient of thermal expansion can be appropriately introduced in a range of about 5% or less.
【００１６】[0016]
【実施例】以下に実施例を例示し本発明を説明する。 〔試料調整〕P2O5源としてオルトリン酸、TeO2源として
二酸化テルル、PbO 源として酸化鉛、ZnO 源として亜鉛
華、BaO 源として炭酸バリウム、Li2O源として炭酸リチ
ウム、Bi2O3 源として酸化ビスマス、Al2O3 源として水
酸化アルミニウム、B2O3源としてほう酸を使用し、ガラ
ス組成換算で表１に示す目標割合で調合し、アルミナ坩
堝に充填後、坩堝に蓋をし、予め1050℃ないし1200℃の
適宜温度に加熱保持した電気炉内にセットし20〜30分間
溶融した。得られた溶融物をいったんカーボンプレート
上に流し出し、さらにこれを電気炉内で徐冷してガラス
試料を得た。The present invention will be described below by way of examples. [Sample preparation] orthophosphoric acid as a source of P 2 O 5 , tellurium dioxide as a source of TeO 2 , lead oxide as a source of PbO, zinc white as a source of ZnO, barium carbonate as a source of BaO, lithium carbonate as a source of Li 2 O, Bi 2 O 3 Using bismuth oxide as a source, aluminum hydroxide as an Al 2 O 3 source, and boric acid as a B 2 O 3 source, they were mixed at the target ratios shown in Table 1 in terms of glass composition, filled in an alumina crucible, and then covered with a lid. Then, it was set in an electric furnace previously heated and maintained at an appropriate temperature of 1050 ° C. to 1200 ° C. and melted for 20 to 30 minutes. The obtained melt was once poured onto a carbon plate, and then gradually cooled in an electric furnace to obtain a glass sample.
【００１７】各成分組成を表１に示す。Table 1 shows the composition of each component.
【００１８】[0018]
【表１】 [Table 1]
【００１９】〔物性測定〕各試料を、シリカガラスを標
準物質とする示差熱膨張計により、昇温速度 5℃／min
の条件で熱膨張を測定し、30〜300 ℃の平均熱膨張率、
ガラス転移点、屈伏点を求めた。別にビッカース微小硬
度計によりビッカース硬度を測定し、また95℃の蒸留水
に20時間浸漬して重量減少率 (耐水性) を求めた。[Measurement of Physical Properties] Each sample was heated at a rate of 5 ° C./min using a differential thermal dilatometer using silica glass as a standard substance.
The thermal expansion was measured under the following conditions.
The glass transition point and the yield point were determined. Separately, Vickers hardness was measured using a Vickers microhardness tester, and the specimen was immersed in distilled water at 95 ° C. for 20 hours to determine the weight loss rate (water resistance).
【００２０】さらに、前記耐水性試験において、測定後
の液中への溶出Pbに関し、塩酸滴下による白濁、白沈
(PbCl2)の生成について観察・定性分析し、白濁、白沈
が認められないもの (○で表示) 、僅かに白沈が認めら
れるもの (△) 、白沈が明白なもの (×) に区分して評
価した。これら物性測定の結果を表１に併せて示す。Further, in the above-mentioned water resistance test, Pb eluted into the liquid after the measurement was examined for turbidity and white precipitate due to dropping of hydrochloric acid.
Observation and qualitative analysis of the formation of (PbCl 2 ) showed that white turbidity and white sediment were not observed (shown by ○), slight white sediment was observed (△), and white sediment was obvious (×). It was evaluated separately. The results of these physical property measurements are also shown in Table 1.
【００２１】〔結果〕 表１において、本発明にかかる実施例1 〜実施例６に対
し、比較例1 は〔ZnO＋BaO ＋Li2O＋Bi2O3 ＋PbO 〕の
和が過剰なケース、比較例2 はTeO2を含まないケース、
比較例3 、4 は先述した公知例に開示されたもので、う
ち比較例3 はPbO が過剰なケース、比較例4 は〔ZnO ＋
BaO ＋Li2O＋Bi2O3 ＋PbO 〕の和が過少なケースを示
す。[0021] In [Results] Table 1, with respect to Examples 1 to 6 according to the present invention, Comparative Example 1 [ZnO + BaO + Li 2 O + Bi 2 O 3 + PbO ] sum excessive case, Comparative Example 2 TeO Case not including 2 ,
Comparative Examples 3 and 4 are disclosed in the above-mentioned known examples, of which Comparative Example 3 is a case where PbO is excessive, and Comparative Example 4 is [ZnO +
The sum of BaO + Li 2 O + Bi 2 O 3 + PbO ] indicates too little case.
【００２２】表示から明らかなとおり、実施例において
はいずれも屈伏点が300 ℃〜400 ℃台半ばと低く、従っ
て接着・封止作業も500 ℃以下ないし600 ℃程度と磁性
材料を損なうようなこともなく、ガラスの熱膨張率は10
0 ×10-7／℃ないし140 ×10 -7／℃台であって、磁性体
材料の熱膨張率に相応して適宜選択・設計でき、ガラス
の耐水性も良好で、Pb溶出も皆無ないし僅少であり、ま
たガラスの硬度も殆どが300 ないし400 台と良好な結果
を示し、他方比較例はガラスの耐水性あるいは更にPb溶
出において劣り、または屈伏点が高い等、磁気ヘッド封
着用として不適当であることを示す。As is clear from the display, in the embodiment,
In all cases, the yield point is as low as about 300 ° C to 400 ° C,
Adhesion and sealing work is less than 500 ℃ to 600 ℃ and magnetic
Without compromising the material, the coefficient of thermal expansion of glass is 10
0x10-7/ ℃ ～ 140 × 10 -7/ ° C, magnetic material
It can be selected and designed as appropriate according to the coefficient of thermal expansion of the material.
Has good water resistance, no or little Pb elution,
Most of the glass has good hardness of 300 to 400 units
On the other hand, the comparative example shows the water resistance of the glass or the Pb solution.
Magnetic head sealing, such as poor in protrusion or high yield point
Indicates that it is inappropriate for wearing.
【００２３】[0023]
【発明の効果】本発明によれば金属、セラミックの接着
・封止用、殊に磁気ヘッドの接着・封止用として有用で
あり、熱膨張率を磁性体のそれと適合させることがで
き、接着・封止温度も磁性体の特性を損なうことのない
作業温度範囲であり、耐水性に優れてPb溶出も皆無ない
し僅少であり、比較的高い硬度を有する等、その工業上
の利用価値は多大である。According to the present invention, the present invention is useful for bonding and sealing metals and ceramics, particularly for bonding and sealing magnetic heads, and can adjust the coefficient of thermal expansion to that of magnetic materials. -The sealing temperature is also within the working temperature range that does not impair the properties of the magnetic material.It has excellent water resistance, no or little Pb elution, and has relatively high hardness. It is.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C03C 1/00 - 14/00 ＣＡ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ)──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 6 , DB name) C03C 1/00-14/00 CA (STN) REGISTRY (STN)
Claims (1)
〜50％、PbO 0 〜＜１％、ZnO 0 〜20％、BaO 0 〜20
％、Li2O 0〜20％、Bi2O3 0 〜10％の範囲で、PbO 、Zn
O 、BaO 、Li2OおよびBi2O3 の和が25〜40％であること
を特徴とする接着・封止用ガラス。(1) In terms of mol%, P 2 O 5 20 to 60%, TeO 2 10
5050%, PbO 0 ＜< 1 %, ZnO 0 2020%, BaO 0 2020
%, Li 2 O 0~20%, in the range of Bi 2 O 3 0 ~10%, PbO, Zn
O, BaO, bonding and sealing glass, wherein the sum of Li 2 O and Bi 2 O 3 is 25 to 40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5271453A JP2987039B2 (en) | 1993-10-29 | 1993-10-29 | Glass for bonding and sealing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5271453A JP2987039B2 (en) | 1993-10-29 | 1993-10-29 | Glass for bonding and sealing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07126037A JPH07126037A (en) | 1995-05-16 |
| JP2987039B2 true JP2987039B2 (en) | 1999-12-06 |
Family
ID=17500245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5271453A Expired - Fee Related JP2987039B2 (en) | 1993-10-29 | 1993-10-29 | Glass for bonding and sealing |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2987039B2 (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7754629B2 (en) * | 2006-11-30 | 2010-07-13 | Corning Incorporated | Phosphotellurite-containing glasses, process for making same and articles comprising same |
| US8308993B2 (en) | 2008-01-30 | 2012-11-13 | Basf Se | Conductive inks |
| US7736546B2 (en) | 2008-01-30 | 2010-06-15 | Basf Se | Glass frits |
| US8383011B2 (en) * | 2008-01-30 | 2013-02-26 | Basf Se | Conductive inks with metallo-organic modifiers |
| GB201407418D0 (en) * | 2014-04-28 | 2014-06-11 | Johnson Matthey Plc | Conductive paste, electrode and solar cell |
| US20200048140A1 (en) * | 2017-02-15 | 2020-02-13 | Basf Se | Glass frit, conductive paste and use of the conductive paste |
| KR102144685B1 (en) * | 2019-03-29 | 2020-08-14 | 전남대학교산학협력단 | Manufacturing method for digital metal-ceramic prosthesis and glass melt bond |
-
1993
- 1993-10-29 JP JP5271453A patent/JP2987039B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07126037A (en) | 1995-05-16 |
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