TW200404752A - Glass frit and method for sealing glass surfaces together - Google Patents

Glass frit and method for sealing glass surfaces together Download PDF

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Publication number
TW200404752A
TW200404752A TW92116419A TW92116419A TW200404752A TW 200404752 A TW200404752 A TW 200404752A TW 92116419 A TW92116419 A TW 92116419A TW 92116419 A TW92116419 A TW 92116419A TW 200404752 A TW200404752 A TW 200404752A
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Taiwan
Prior art keywords
glass
sealing
paste
patent application
item
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TW92116419A
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Chinese (zh)
Inventor
Oliver Steigelmann
Ton Reinier Mulderij
Hal Henricus Albertus Maria Van
Wilhelmus Cornelis Keur
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Koninkl Philips Electronics Nv
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Publication of TW200404752A publication Critical patent/TW200404752A/en

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    • 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
    • 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
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06—Joining glass to glass by processes other than fusing
    • 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
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • 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
    • 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
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Glass Compositions (AREA)
  • Manufacture Of Electron Tubes, Discharge Lamp Vessels, Lead-In Wires, And The Like (AREA)

Abstract

Disclosed is a glass frit suitable for sealing glass surfaces together, said glass frit comprising lead oxide. The glass frit further comprises an oxidizing agent selected from the group of higher valent oxides comprising manganates (VII), manganates (VI) and ferrate (VI). Also described is a sealing glass paste comprising at least such a glass frit and a vehicle. Moreover a method for sealing two glass surfaces together is disclosed. Said method at least comprises the steps of: - providing a first and a second glass surface; - applying an amount of the above sealing glass paste on at least one of said surfaces; - placing the glass surfaces against each other with the sealing glass paste in-between; - subjecting the assembly of glass surfaces and sealing paste to a temperature sufficient to fuse the sealing glass paste on both glass surfaces, thereby sealing the two surfaces together; and - cooling the resulting sealed assembly.

Description

200404752 玖、發明說明·· 【發明所屬之技術領域】 發明係關於-種玻璃焊料，4用於將破璃表面 :錢璃焊料包含氧化錯。再者，本發明係關：―種 :起二J含此-玻璃糊…種將兩個破璃表面密封在 【先前技術】 破璃焊料可用來將玻璃表面密封在一起。至今 :糊是以破璃焊料製成的，藉著將峨料粉末與：合劑 岭:夜或媒介物混合。玻璃焊料粉末之使用的—個已熟知實 例被發現在陰極射線管的製造上’其中crt的面板及狹窄處 使用玻璃焊料被密封在—起。為了降低crt密封所 :的概度，衩佳使用包含高Pb0含量的玻璃焊料。然而高扑〇 ，量導致高Pb還原的趨勢及金屬鉛的形成。金屬鉛的存在 是不利的，因其影響玻璃焊料黏合及密封物的導電性質。 美國US A-j，973,975號處理上述的問題，並且揭示在密封 玻璃糊焊料中加入一種陽離子較高氧化物的粉末，以避免 PbO還原。當其曝露於還原條件下時，陽離子的較高氧化物 可被還原成陽離子的較低氧化物。該陽離子之較高氧化物 是選 i Pb3〇4、Ba〇2、Mn〇2、Mn2〇3、Fe3〇4、Cu〇、Cu2〇 、T1203、Te〇2、Ta2〇5、Nb2〇5、V2〇5、Ce〇2及 Bi203 所組成 的族群。 然而’為了避免Pb〇還原所添加之陽離子較高氧化物的份 里是相當高的。再者，較高陽離子氧化物只在還原條件下 86128 200404752 還原成相對應之較低陽離子氧化物。 【發明内容】 本發明目標是根據前述提供一種玻璃焊料，其避免存在 於該玻璃焊料中的Pb〇還原，並且克服上述的問題。 至此，本發明的特徵在於：該玻璃焊料進_步包含氧化劑 ’是選自較高價數的氧化物族群，包含鐘酸鹽（VII)、猛酸 鹽（VI)及高鐵酸鹽（VI)。 此類氧化劑在存在於密封玻璃糊中之黏合劑的燃燒溫度 下產生氧氣，因此，避免pb0還原成金屬鉛。要強調的是： 還原條件對產生氧氣不是必要的。根據本發明之有氧化劑 玻璃焊料的另一個優點是在密封邊緣的有機污染物更有效 地被燒掉，是由於由氧化劑產生之氧的存在。 較佳地，該氧化劑被定義為x(Mn04),其中x是選自Na、 K、Cs、Ba、Sr、Ca、Mg或Zn所組成之族群的元素。 特佳的化合物是BaMn04。 該化合物已證明特別有用地做為氧化劑。上述物質的特 力1J優點疋在咸玻璃’焊料中無新物質被導入。 優越地，該玻璃焊料只包含0·02至〇.8重量％的氧化劑，以 玻璃绛料粉末的總量為基礎。較佳地，該破璃焊料只包含 〇 · 0 5至0 · 5重量％的氧化劑。 當上述的氧化劑提供相當高份量的氧時，在一般加工條200404752 发明 Description of the invention ... [Technical field to which the invention belongs] The invention relates to a kind of glass solder, 4 is used to break the surface of the glass: money glass solder contains oxidation faults. In addition, the present invention relates to: ―species: from the second to the second, the glass paste, etc.‖, which seals the two broken glass surfaces in [prior art] The broken glass solder can be used to seal the glass surfaces together. So far: the paste is made of broken glass solder, by mixing the E material powder with: Mixture Ridge: Night or vehicle. A well-known example of the use of glass solder powder is found in the manufacture of cathode ray tubes, in which the panel and the narrow area of crt are sealed with glass solder. In order to reduce the probability of crt sealing, the best use of glass solder containing high Pb0 content. However, high flutter, the amount leads to the trend of high Pb reduction and the formation of metallic lead. The presence of metallic lead is disadvantageous because it affects the soldering properties of the glass solder and the conductive properties of the seal. US A-j, 973,975 addresses the above problems and discloses the addition of a cationic higher oxide powder to the sealing glass paste solder to avoid PbO reduction. When exposed to reducing conditions, higher cation oxides can be reduced to lower cation oxides. The higher oxides of this cation are selected from the group consisting of Pb304, Ba02, Mn02, Mn203, Fe304, CuO, Cu20, T1203, Te02, Ta205, Nb205, V205, Ce02 and Bi203. However, the proportion of higher cation oxides added to avoid PbO reduction is quite high. Furthermore, higher cationic oxides are reduced to the corresponding lower cationic oxides only under reducing conditions. SUMMARY OF THE INVENTION The object of the present invention is to provide a glass solder according to the foregoing, which avoids the reduction of Pb0 existing in the glass solder and overcomes the above-mentioned problems. So far, the present invention is characterized in that the glass solder further contains an oxidant ′ which is selected from a group of oxides having a higher valence, and includes bellate (VII), ferrate (VI), and ferrate (VI). This type of oxidant generates oxygen at the combustion temperature of the binder present in the sealing glass paste, thus avoiding the reduction of pb0 to metallic lead. It is emphasized that the reducing conditions are not necessary for the production of oxygen. Another advantage of the oxidized glass solder according to the present invention is that the organic contaminants at the sealing edges are more effectively burned due to the presence of oxygen generated by the oxidant. Preferably, the oxidant is defined as x (Mn04), where x is an element selected from the group consisting of Na, K, Cs, Ba, Sr, Ca, Mg or Zn. A particularly preferred compound is BaMn04. This compound has proven to be particularly useful as an oxidant. Advantages of the above-mentioned special substance 1J: No new substance is introduced into the salty glass' solder. Advantageously, the glass solder contains only 0.02 to 0.8% by weight of an oxidizing agent, based on the total amount of glass frit powder. Preferably, the glass-breaking solder contains only 0.05 to 0.5% by weight of an oxidizing agent. When the above oxidants provide a relatively high amount of oxygen,

件下， 屬鉛。 污染物 86128 200404752Under the lead, it belongs to lead. Contaminants 86128 200404752

PbO份量是至少75重量％。 争別^在Pb〇份I南於75重量〇/〇時，PbO還原的問題會 發生。猎著添加根據本發明的氧化劑，該問題被避免。 本發明進—步係關於-種密封玻璃糊，#包含至少…種 根據本發明的玻璃焊料及媒介物。 為了使用破璃焊料將破璃表面密封在一起，首先密封玻 璃糊必須以破璃焊料製成，是藉著將該玻璃弹料與i當媒 介物混合。 、該媒介物可為一種以硝基纖維素或戊基-/或丁基醋酸酯 為基礎的有機黏合劑，其在低溫時被燒掉。此黏合劑的一 個缺點是其導致環境問題，並且叫存在為終產物。 為了克服該問題，該媒介物優越地包含纖維素醚的水溶 液。 當使用此水性媒介物時，可使用在玻璃焊料中以氧化劑 產生之氧，以輔助媒介物的完全燃燒。 最後，本發明係關於一種將兩個玻璃表面密封在一起的 方法’至少包含下列步驟·· -提供第一及第二玻璃表面； -將含封玻璃糊的份量加到至少一個該表面上· -將該破璃表面互相置放在一起，有該密封破璃糊在其間； -對玻璃表面的組合及密封糊加上足以融合在兩個玻璃表 面上之密封玻璃糊的溫度，因此將兩個表面密封在一起· 及 -冷卻所得之經密封的組合。 86128 200404752 明之密封 ，同時第 該方法的特徵在於··該密封玻璃糊包含根據本發 玻璃糊。 特別地，第一玻璃表面包含陰極射線管的面板 破璃表面包含陰極射線管的狹窄處（funnel)部分。 86128The PbO portion is at least 75% by weight. Say goodbye. When the PbO content is less than 75% by weight, the problem of PbO reduction will occur. This problem is avoided by hunting the addition of an oxidant according to the invention. The invention further relates to a kind of sealing glass paste, which contains at least ... a glass solder and a medium according to the invention. In order to seal the broken glass surfaces together using the broken glass solder, the sealing glass paste must first be made of broken glass solder by mixing the glass spring with i as a medium. The vehicle may be an organic binder based on nitrocellulose or pentyl- / or butyl acetate, which is burned off at low temperatures. One disadvantage of this adhesive is that it causes environmental problems and is called presence as an end product. To overcome this problem, the vehicle advantageously contains an aqueous solution of cellulose ether. When using this aqueous vehicle, it is possible to use oxygen generated by oxidizing agents in glass solders to assist in the complete combustion of the vehicle. Finally, the present invention relates to a method of sealing two glass surfaces together, which includes at least the following steps:-providing a first and a second glass surface;-adding a portion of the sealing glass paste to at least one of the surfaces. -Put the broken glass surfaces on each other with the sealing broken glass paste in between;-add the temperature of the sealing glass paste to the combination of the glass surface and the sealing paste sufficient to fuse the two glass surfaces, so the two The two surfaces are sealed together and the sealed combination obtained by cooling. 86128 200404752, and the method is characterized in that the sealing glass paste contains the glass paste according to the present invention. In particular, the first glass surface includes a panel of a cathode ray tube, and the broken glass surface includes a narrow section of the cathode ray tube. 86128

Claims (1)

200404752 拾、申請專利範圍： 1·-種適用於將玻璃表面密封在_起的破璃焊料，該破璃 焊料包含氧化鉛，其特徵在於：在該玻璃焊料中進一步包 含氧化劑’是選自較高價數之氧化物的族群，包含錳酸 鹽（VI1)、鐘酸鹽（VI)及高鐵酸鹽（VI)。 2.如申請專利範圍第i項的玻璃焊料，其特徵在於：該氧化 劑被定義為Χ(Μη04)，其中X是選自Na、K、Cs、Ba、 Sr、Ca、Mg或Zn所組成之族群的元素。 3·如申請專利範圍第丨或2項的玻璃焊料，其特徵在於：其包 含0.02至0.8重量％的氧化劑，以玻璃坪料粉末的總量為 基礎。 4·如申請專利範圍第3項的玻璃焊料，其特徵在於：其包含 0.05至0.5重量％的氧化劑，以破璃焊料粉末的總量為基 礎。 5. 如申請專利範圍第1項的玻璃焊料，其特徵在於：其包含 的Pb〇份量是至少75重量％。 6. 一種密封玻璃糊，包含至少一種根據申請專利範圍第i _ 5 項之任一項的玻璃焊料及一種媒介物。 7. 如申請專利範圍第6項的密封玻璃糊，其特徵在於：該媒 介物包含纖維素醚的水溶液。 8 · 一種將兩個破璃表面密封在一起的方法，至少包含下列 步驟： *才疋供弟一及弟二玻璃表面； -將密封破璃糊的份量加到至少一個該表面上； 斗 /52 將該破璃表面互相置放在一起，有該密封玻璃糊在 一對玻璃表面的組合及密封糊加上足以融合在兩個 皮璃表面上之密封玻璃糊的溫度，因此將兩個表面密封 在一起；及 " 冷卻所得之經密封的組合， 其特徵在於：該密封玻璃糊包含根據申請專利範圍第7 或8項的密封玻璃糊。 9.根據申請專利範圍第8項的方法，其特徵在於：第一玻璃 表面包含陰極射線管的面板，同時第二玻璃表面包含陰 極射線管的狹窄處（funnel)部分。 86128 200404752 柒、指定代表圖： (一) 本案指定代表圖為：第（無）圖。 (二) 本代表圖之元件代表符號簡單說明： 捌、本案若有化學式時，請揭示最能顯示發明特徵的化學式： 86128200404752 Scope of patent application: 1 · A kind of broken glass solder suitable for sealing the glass surface. The broken glass solder contains lead oxide, which is characterized in that the glass solder further contains an oxidizing agent. The high-valence oxide group includes manganate (VI1), bellate (VI), and ferrate (VI). 2. The glass solder according to item i of the patent application scope, characterized in that the oxidant is defined as X (Μη04), where X is a composition selected from Na, K, Cs, Ba, Sr, Ca, Mg or Zn Ethnic elements. 3. The glass solder according to item 1 or 2 of the scope of patent application, characterized in that it contains 0.02 to 0.8% by weight of an oxidizing agent, based on the total amount of glass mat powder. 4. The glass solder according to item 3 of the patent application scope, characterized in that it contains 0.05 to 0.5% by weight of an oxidizing agent, based on the total amount of the glass-breaking solder powder. 5. The glass solder according to item 1 of the patent application range, characterized in that it contains at least 75% by weight of Pb. 6. A sealing glass paste comprising at least one glass solder according to any one of items i_5 of the scope of patent application and a vehicle. 7. The sealed glass paste according to item 6 of the scope of patent application, characterized in that the medium comprises an aqueous solution of cellulose ether. 8 · A method of sealing two broken glass surfaces together, including at least the following steps: * Only for the first and second glass surfaces;-adding the amount of sealing glass paste to at least one of the surfaces; bucket / 52 Put the broken glass surfaces on each other, there is a combination of the sealing glass paste on a pair of glass surfaces and the temperature of the sealing paste plus the sealing glass paste sufficient to fuse the two glass surfaces, so the two surfaces Sealed together; and " a sealed combination obtained by cooling, characterized in that the sealing glass paste comprises a sealing glass paste according to item 7 or 8 of the scope of patent application. 9. The method according to item 8 of the patent application, characterized in that the first glass surface includes a panel of a cathode ray tube, and the second glass surface includes a narrow portion of a cathode ray tube. 86128 200404752 (1) Designated representative map: (1) The designated representative map in this case is: (none) map. (2) Brief description of the representative symbols of the elements in this representative diagram: 捌 If there is a chemical formula in this case, please disclose the chemical formula that can best show the characteristics of the invention: 86128
TW92116419A 2002-06-20 2003-06-17 Glass frit and method for sealing glass surfaces together TW200404752A (en)

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AU (1) AU2003236995A1 (en)
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005044523A1 (en) * 2005-09-16 2007-03-29 Schott Ag Connecting elements using a glass solder used in the manufacture of electronic components comprises soldering the elements together by fusing a glass solder and releasing the oxidant locally during soldering
US20080226863A1 (en) * 2007-03-16 2008-09-18 Robert Prunchak Glass Enamel Screen Printing Composition
US8147632B2 (en) * 2008-05-30 2012-04-03 Corning Incorporated Controlled atmosphere when sintering a frit to a glass plate
PT104282A (en) 2008-12-05 2010-06-07 Univ Do Porto DSC SOLAR CELL GLASS SELECTION PROCESS
DE102008063636A1 (en) * 2008-12-18 2010-06-24 Osram Opto Semiconductors Gmbh Method for producing an organic optoelectronic component and organic optoelectronic component
KR20140134565A (en) 2013-05-14 2014-11-24 삼성디스플레이 주식회사 Display apparatus and method for manufacturing the same
KR102078356B1 (en) 2013-05-16 2020-04-08 삼성디스플레이 주식회사 Organic light emitting display apparatus and manufacturing method thereof
CN117276383B (en) * 2023-11-21 2024-02-27 天合光能股份有限公司 Photovoltaic module and sealing method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3973975A (en) * 1972-04-21 1976-08-10 Owens-Illinois, Inc. PbO-containing sealing glass with higher oxide of a cation to avoid PbO reduction
GB9713831D0 (en) * 1997-06-30 1997-09-03 Fry Metals Inc Sealing glass paste for cathode ray tubes

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AU2003236995A1 (en) 2004-01-06
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CN1662461A (en) 2005-08-31
WO2004000745A1 (en) 2003-12-31

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