JPH0769670A - Glass material for sealing - Google Patents

Glass material for sealing

Info

Publication number
JPH0769670A
JPH0769670A JP22081093A JP22081093A JPH0769670A JP H0769670 A JPH0769670 A JP H0769670A JP 22081093 A JP22081093 A JP 22081093A JP 22081093 A JP22081093 A JP 22081093A JP H0769670 A JPH0769670 A JP H0769670A
Authority
JP
Japan
Prior art keywords
glass
sealing
powder
titanate
cordierite
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Withdrawn
Application number
JP22081093A
Other languages
Japanese (ja)
Inventor
Takashi Sunada
貴 砂田
Hiroyuki Tanaka
弘之 田中
Toshio Akimoto
俊夫 秋元
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Sheet Glass Co Ltd
Original Assignee
Nippon Sheet Glass Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Sheet Glass Co Ltd filed Critical Nippon Sheet Glass Co Ltd
Priority to JP22081093A priority Critical patent/JPH0769670A/en
Publication of JPH0769670A publication Critical patent/JPH0769670A/en
Withdrawn legal-status Critical Current

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
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
    • C03C3/072—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron
    • C03C3/074—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron containing zinc
    • C03C3/0745—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron containing zinc containing more than 50% lead oxide, by weight
    • 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

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

PURPOSE:To obtain a sealing glass excellent in durability under conditions of high temp., high humidity, and high voltage. CONSTITUTION:This sealing glass consists of a mixture powder obtd. by mixing a crystal powder of cordierite, titanate or zircon with a glass powder. The compsn. of the glass powder consists of 75-85wt.% PbO, 8-13wt.% B2O3, 3-8wt.% SiO2, 2-7wt.% ZnO, and 1-4wt.% Al2O3. The compsn. of the mixture powder consists of 60-92wt.% glass powder, 2-15wt.% of zircon, 0-15wt.% cordierite, and 0-25wt.% titanate. When both of cordierite and titanate are added, the sum of these is specified to 4-25wt.%.

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【産業上の利用分野】本発明はブラウン管等の各種ディ
スプレイ材料の封着やＩＣ用のアルミナパッケージ等の
封着に用いるガラス材料に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a glass material used for sealing various display materials such as cathode ray tubes and alumina packages for ICs.

【０００２】[0002]

【従来の技術】ガラス、セラミック或いは金属材料を気
密に封着する封着用ガラスとして、従来からＰbＯ−Ｂ2
Ｏ3−ＳiＯ2−Ａl2Ｏ3系の非結晶性低融点ガラス、或い
はＰbＯ−ＺnＯ−Ｂ2Ｏ3−ＳiＯ2系の結晶性低融点ガラ
スが一般的に用いられているが、これらを更に改善した
封着用ガラスとして、特開昭４９−２４２０８号公報、
特開昭５２−５６８６７号公報、特公昭６２−４７８２
４号公報等に開示されるものが知られている。2. Description of the Related Art PbO-B 2 has hitherto been used as a sealing glass for hermetically sealing glass, ceramic or metal materials.
O 3 --SiO 2 --Al 2 O 3 type amorphous low melting point glass or PbO--ZnO--B 2 O 3 --SiO 2 type crystalline low melting point glass is generally used. Further improved glass for sealing is disclosed in JP-A-49-24208.
JP-A-52-56867, JP-B-62-4782
Those disclosed in Japanese Patent Publication No. 4 and the like are known.

【０００３】特開昭４９−２４２０８号公報に開示され
る封着ガラスは、低融点ガラスにβ−ユークリプタイ
ト、β−スポジューメン、チタン酸塩、石英またはジル
コン等を添加して、低温（４５０℃以下）での封着ガラ
スの膨張係数を小さくし、被封着材の膨張係数に近づけ
るようにしたものであり、同様の封着用ガラスとして米
国特許第３２５０６３１号公報、米国特許第３２５８３
５０号公報に開示されるものがある。The sealing glass disclosed in Japanese Unexamined Patent Publication No. 49-24208 is a low melting point glass prepared by adding β-eucryptite, β-spodumene, titanate, quartz or zircon to a low temperature (450 The expansion coefficient of the sealing glass at (° C. or lower) is made small so as to be close to the expansion coefficient of the material to be sealed. Similar sealing glass is disclosed in US Pat. No. 3,250,631 and US Pat. No. 32583.
There is one disclosed in Japanese Patent Laid-Open No. 50.

【０００４】特開昭５２−５６８６７号公報に開示され
る封着用ガラスは、ＰbＯ−ＺnＯ−Ｂ2Ｏ3−ＳiＯ2−Ａ
l2Ｏ3系の低融点ガラスに所定割合でコージェライト及
びチタン酸塩を添加し、硫酸含有の電解錫メッキ浴に対
して化学的耐性を有するようにしたものであり、同様に
コージェライトを添加した封着用ガラスとして特開昭５
６−６９２４２号公報、特公昭６１−４３２９８号公報
に開示されるものがあり、チタン酸塩とジルコンを含有
させることでメッキ工程での酸に侵されにくくしたもの
が特公昭５４−２３９２８に開示されている。[0004] sealing glass disclosed in JP-52-56867 Publication, PbO-ZnO-B 2 O 3 -SiO 2 -A
Cordierite and titanate were added to a low melting point glass of l 2 O 3 system at a predetermined ratio so as to have chemical resistance to an electrolytic tin plating bath containing sulfuric acid. As the added glass for sealing, Japanese Patent Laid-Open No. Sho 5
6-69242 and JP-B-61-43298, and JP-B-54-23928 discloses one containing titanate and zircon to make it less susceptible to acid in the plating process. Has been done.

【０００５】特公昭６２−４７８２４号公報に開示され
る封着用ガラスは、ＰbＯ−Ｂ2Ｏ3−ＳiＯ2−Ａl2Ｏ3系
の低融点ガラスにジルコンを添加することによって直流
電圧を印加しても黒化しないようにしたものである。The glass for sealing disclosed in Japanese Patent Publication No. 62-47824 is a PbO-B 2 O 3 -SiO 2 -Al 2 O 3 -based low melting glass to which a DC voltage is applied by adding zircon. Even so, it does not turn black.

【０００６】[0006]

【発明が解決しようとする課題】上述した従来の封着用
ガラスはいずれも４５０℃以下の温度での封着が可能
で、流動性及び被封着材とのなじみも良好であるが、β
−ユークリプタイト及びβ−スポジューメンは組成的に
アルカリ（リチウム）を含み、体積抵抗率が小さくな
り、フラットＣＲＴ等の封着には適さない。また、上述
した従来の封着用ガラスは機械的耐圧性及び高温高湿下
で高電圧を印加した場合の化学的耐性に劣る。また、従
来の封着用ガラスはＳiＯ2の割合が多く、耐水、耐湿性
が悪くなりやすい。All of the conventional sealing glasses described above can be sealed at a temperature of 450 ° C. or lower, and have good fluidity and good compatibility with the material to be sealed.
-Eucryptite and β-spodumene compositionally contain alkali (lithium), have a low volume resistivity, and are not suitable for sealing flat CRTs and the like. Further, the above-mentioned conventional sealing glass is inferior in mechanical pressure resistance and chemical resistance when a high voltage is applied under high temperature and high humidity. Further, the conventional glass for sealing has a large proportion of SiO 2 and is likely to have poor water resistance and moisture resistance.

【０００７】[0007]

【課題を解決するための手段】上記課題を解決すべく本
発明は、ガラス粉末にコージェライト、チタン酸塩また
はジルコンの結晶粉末を混合した混合粉末からなる封着
用ガラスにおいて、前記ガラス粉末及び前記混合粉末は
以下の組成割合からなるものとした。 ガラス粉末 ＰbＯ：７５〜８５重量％ Ｂ2Ｏ3：８〜１３重量％ ＳiＯ2：３〜８重量％ ＺnＯ：２〜７重量％ Ａl2Ｏ3：１〜４重量％ 混合粉末 ガラス粉末：６０〜９２重量％ ジルコン：２〜１５重量％ コージェライト：０〜１５重量％ チタン酸塩：０〜２５重量％ 但し、コージェライトとチタン酸塩とを添加する場合に
はこれらの合計で４〜２５重量％とする。Means for Solving the Problems To solve the above problems, the present invention relates to a sealing glass comprising a mixed powder of glass powder and crystal powder of cordierite, titanate or zircon. The mixed powder had the following composition ratios. Glass powder PbO: 75-85 wt% B 2 O 3: 8 to 13 wt% SiO 2: 3 to 8 wt% ZnO: 2 to 7 wt% Al 2 O 3: 1 to 4 wt% mixed powdered glass powder: 60 -92 wt% Zircon: 2-15 wt% Cordierite: 0-15 wt% Titanate: 0-25 wt% However, when cordierite and titanate are added, the total of these is 4-25. Weight%

【０００８】ガラス粉末を構成する各材料の組成割合を
上記にした理由を以下に述べる。ＰbＯについては、７
５重量％未満であると４５０℃以下での封着が困難にな
り、８５重量％を超えるとガラスが失透したり耐水、耐
湿性が悪くなる。Ｂ2Ｏ3については、８重量％未満であ
るとガラスが失透しやすくなり、１３重量％を超えると
４５０℃以下での封着が困難になる。ＳiＯ2について
は、３重量％未満であると耐水、耐湿性が悪くなり、８
重量％を超えるとフリットとしての流動性が悪くなり、
４５０℃以下での封着が困難になる。ＺnＯについて
は、２重量％未満であると耐水、耐湿性が悪くなり強度
が低下し、７重量％を超えるとフリット焼成時に結晶化
して流動性が悪くなる。Ａl2Ｏ3については、１重量％
未満であると耐水、耐湿性が悪くなり、４重量％を超え
るとガラスが失透しやすくなる。The reason why the composition ratio of each material constituting the glass powder is set to the above is described below. 7 for PbO
If it is less than 5% by weight, sealing at 450 ° C. or less becomes difficult, and if it exceeds 85% by weight, the glass becomes devitrified and water resistance and moisture resistance deteriorate. If B 2 O 3 is less than 8% by weight, the glass tends to devitrify, and if it exceeds 13% by weight, sealing at 450 ° C. or lower becomes difficult. With respect to SiO 2, if it is less than 3% by weight, water resistance and moisture resistance deteriorate, and
When it exceeds the weight%, the fluidity as a frit becomes poor,
Sealing at 450 ° C or lower becomes difficult. If ZnO is less than 2% by weight, water resistance and moisture resistance are deteriorated and the strength is lowered, and if it exceeds 7% by weight, crystallization occurs during frit firing, resulting in poor fluidity. Al 2 O 3 is 1% by weight
If it is less than 4% by weight, water resistance and moisture resistance are poor, and if it exceeds 4% by weight, the glass tends to devitrify.

【０００９】ガラス粉末に添加するジルコン、コージェ
ライト、チタン酸塩の組成割合を上記にした理由を以下
に述べる。ジルコンについては、２重量％未満であると
強度が不足し、１５重量％を超えると流動性が悪くな
る。コージェライトについては、１５重量％を超えると
膨張係数が小さくなりすぎる。チタン酸塩については、
２５重量％を超えると膨張係数が小さくなりすぎる。ま
た、コージェライトとチタン酸塩とを添加する場合につ
いては、４重量％未満であると膨張係数が大きくなり、
２５重量％を超えると膨張係数が小さくなりすぎる。The reason why the composition ratios of zircon, cordierite and titanate added to the glass powder are set as above will be described below. With respect to zircon, if it is less than 2% by weight, the strength is insufficient, and if it exceeds 15% by weight, the fluidity becomes poor. For cordierite, if it exceeds 15% by weight, the expansion coefficient becomes too small. For titanates,
If it exceeds 25% by weight, the expansion coefficient becomes too small. Further, in the case of adding cordierite and titanate, if it is less than 4% by weight, the expansion coefficient becomes large,
If it exceeds 25% by weight, the expansion coefficient becomes too small.

【００１０】[0010]

【作用】ガラス粉末の構成材料の組成割合およびこれに
添加する材料の割合を適正なものとすることで、高温、
高湿、高電圧の条件下でも耐久性に優れた封着用ガラス
が得られる。[Function] By making the composition ratio of the constituent materials of the glass powder and the ratio of the material added to the glass powder proper, the high temperature,
It is possible to obtain a glass for sealing which has excellent durability even under conditions of high humidity and high voltage.

【００１１】[0011]

【実施例】以下の（表１）に示す組成割合で調合した原
料を白金坩堝に入れ、１０００〜１２００℃で１〜２時
間溶融する。次いで、溶融したガラスを水砕し、ボール
ミルで１００μｍ以下に粉砕する。この粉末ガラスに１
００μｍ以下に粉砕したフィラー（無機結晶の充填剤）
を加えて均質に混合し、本発明及び比較例の封着用ガラ
スとした。上記の封着用ガラスにビークル（ニトロセル
ロースを酢酸イソアミル溶液で溶かしたもの）を適量混
合してペースト状にし、これをフラットＣＲＴ等の接着
面に塗布し、ボタンフロー径、熱膨張係数及び耐水性を
評価した。[Examples] Raw materials prepared in the following compositional ratios (Table 1) were put into a platinum crucible and melted at 1000 to 1200 ° C for 1 to 2 hours. Next, the molten glass is granulated with water and crushed with a ball mill to 100 μm or less. 1 for this powdered glass
Filler crushed to less than 00 μm (filler of inorganic crystals)
Was added and mixed homogeneously to obtain the glass for sealing of the present invention and the comparative example. A suitable amount of vehicle (nitrocellulose dissolved in isoamyl acetate solution) is mixed into the above sealing glass to form a paste, which is applied to the adhesive surface of a flat CRT, etc., and has a button flow diameter, thermal expansion coefficient and water resistance. Was evaluated.

【００１２】[0012]

【表１】 [Table 1]

【００１３】また、ボタンフロー径、熱膨張係数及び耐
水性の評価は以下のようにして行った。 （ボタンフロー径）封着用ガラス粉末１０ｇを秤量し、
これを直径１２．５ｍｍの円盤状にプレス成形する（プ
レス圧力約１０００Ｋｇ／ｃｍ2）。これをソーダ石灰
ガラス板の上において、４５０℃で１時間焼成する。通
常サンプルは軟化流動し、ほぼ円盤状に広がる。この円
盤の直径をもってフロー径とし、流動性の尺度とする。
経験的にフロー径が２５ｍｍ以上であれば、おおむね良
好な接着が可能である。 （熱膨張係数）熱膨張計を用いて測定し、３０℃〜ガラ
ス転移点までの平均の値で表わした。 （耐水性）封着用ガラスをソーダ石灰ガラスに塗布して
焼成し、耐水試験用サンプルを得る。これを８０℃の温
水中に浸漬し、２４時間後に取り出す。サンプルの表面
を観察し、温水による侵食に対する抵抗を評価した。The button flow diameter, thermal expansion coefficient and water resistance were evaluated as follows. (Button flow diameter) Weigh 10 g of glass powder for sealing,
This is press-molded into a disk having a diameter of 12.5 mm (pressing pressure of about 1000 Kg / cm 2 ). This is baked on a soda-lime glass plate at 450 ° C. for 1 hour. Normally, the sample softens and flows, and spreads out in a substantially disc shape. The diameter of this disk is used as the flow diameter and is used as a measure of fluidity.
Empirically, if the flow diameter is 25 mm or more, generally good adhesion is possible. (Coefficient of thermal expansion) The coefficient of thermal expansion was measured using a thermal dilatometer and expressed as an average value from 30 ° C to the glass transition point. (Water resistance) A glass for sealing is applied to soda lime glass and baked to obtain a water resistance test sample. This is immersed in warm water of 80 ° C. and taken out after 24 hours. The surface of the sample was observed and evaluated for resistance to erosion by hot water.

【００１４】[0014]

【発明の効果】（表１）に示した結果から明らかなよう
に、本発明にかかる封着用ガラス材料は、全てボタンフ
ロー径が２５ｍｍを越えており、流動性に優れているこ
とが分る。また、熱膨張係数もフラットＣＲＴ等の接着
に適した範囲に収まっており、更に耐水性においても優
れている。特に耐水性については、サンプル８と比較例
１のものを８０℃の温水に２４時間浸漬した時の単位面
積あたりの各成分の溶出量の合計を測定したところ、比
較例１の１７００ｍｇ／ｃｍ2に対し、サンプル８は３
４０ｍｇ／ｃｍ2であり、大幅に耐水性が向上してい
た。As is clear from the results shown in (Table 1), all the glass materials for sealing according to the present invention have a button flow diameter of more than 25 mm and are excellent in fluidity. . Also, the coefficient of thermal expansion is within a range suitable for adhesion of flat CRT and the like, and is also excellent in water resistance. Particularly with respect to water resistance, when the sample 8 and the sample of Comparative Example 1 were immersed in hot water at 80 ° C. for 24 hours, the total elution amount of each component per unit area was measured, and the result was 1700 mg / cm 2 of Comparative Example 1. On the other hand, sample 8 is 3
It was 40 mg / cm 2 , and the water resistance was significantly improved.

Claims (1)

【特許請求の範囲】[Claims] 【請求項１】 ガラス粉末にコージェライト、チタン酸
塩またはジルコンの結晶粉末を混合した混合粉末からな
る封着用ガラスにおいて、前記ガラス粉末及び前記混合
粉末は以下の組成割合からなることを特徴とする封着用
ガラス材料。 ガラス粉末 ＰbＯ：７５〜８５重量％ Ｂ2Ｏ3：８〜１３重量％ ＳiＯ2：３〜８重量％ ＺnＯ：２〜７重量％ Ａl2Ｏ3：１〜４重量％ 混合粉末 ガラス粉末：６０〜９２重量％ ジルコン：２〜１５重量％ コージェライト：０〜１５重量％ チタン酸塩：０〜２５重量％ 但し、コージェライトとチタン酸塩とを添加する場合に
はこれらの合計で４〜２５重量％とする。1. A sealing glass comprising a mixed powder obtained by mixing crystal powder of cordierite, titanate or zircon with glass powder, wherein the glass powder and the mixed powder have the following composition ratios. Glass material for sealing. Glass powder PbO: 75-85 wt% B 2 O 3: 8 to 13 wt% SiO 2: 3 to 8 wt% ZnO: 2 to 7 wt% Al 2 O 3: 1 to 4 wt% mixed powdered glass powder: 60 -92 wt% Zircon: 2-15 wt% Cordierite: 0-15 wt% Titanate: 0-25 wt% However, when cordierite and titanate are added, the total of these is 4-25. Weight%
JP22081093A 1993-09-06 1993-09-06 Glass material for sealing Withdrawn JPH0769670A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22081093A JPH0769670A (en) 1993-09-06 1993-09-06 Glass material for sealing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22081093A JPH0769670A (en) 1993-09-06 1993-09-06 Glass material for sealing

Publications (1)

Publication Number Publication Date
JPH0769670A true JPH0769670A (en) 1995-03-14

Family

ID=16756921

Family Applications (1)

Application Number Title Priority Date Filing Date
JP22081093A Withdrawn JPH0769670A (en) 1993-09-06 1993-09-06 Glass material for sealing

Country Status (1)

Country Link
JP (1) JPH0769670A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0828693A4 (en) * 1996-04-02 1998-11-18 Techneglas Inc Sealing glass modifier for use with voc-free or low-voc vehicle
KR100376283B1 (en) * 1995-12-15 2003-06-11 삼성코닝 주식회사 Adhesive glass composition
US6583079B1 (en) * 1999-02-19 2003-06-24 Nippon Electric Glass Co., Ltd. CRT frit capable of sealing a CRT bulb at a relatively low temperature and in a short time
JP2008303075A (en) * 2007-06-05 2008-12-18 Central Glass Co Ltd Insulating coating material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100376283B1 (en) * 1995-12-15 2003-06-11 삼성코닝 주식회사 Adhesive glass composition
EP0828693A4 (en) * 1996-04-02 1998-11-18 Techneglas Inc Sealing glass modifier for use with voc-free or low-voc vehicle
US6583079B1 (en) * 1999-02-19 2003-06-24 Nippon Electric Glass Co., Ltd. CRT frit capable of sealing a CRT bulb at a relatively low temperature and in a short time
JP2008303075A (en) * 2007-06-05 2008-12-18 Central Glass Co Ltd Insulating coating material

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