JPH0411511B2 - - Google Patents
Info
- Publication number
- JPH0411511B2 JPH0411511B2 JP13006484A JP13006484A JPH0411511B2 JP H0411511 B2 JPH0411511 B2 JP H0411511B2 JP 13006484 A JP13006484 A JP 13006484A JP 13006484 A JP13006484 A JP 13006484A JP H0411511 B2 JPH0411511 B2 JP H0411511B2
- Authority
- JP
- Japan
- Prior art keywords
- weight
- sealing
- ceramic
- sealing material
- arc tube
- 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
- 238000007789 sealing Methods 0.000 claims description 14
- 239000000919 ceramic Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000003566 sealing material Substances 0.000 description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 9
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 9
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 229910001507 metal halide Inorganic materials 0.000 description 9
- 150000005309 metal halides Chemical class 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 229910052736 halogen Inorganic materials 0.000 description 6
- 150000002367 halogens Chemical class 0.000 description 6
- 238000009877 rendering Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- GQKYKPLGNBXERW-UHFFFAOYSA-N 6-fluoro-1h-indazol-5-amine Chemical compound C1=C(F)C(N)=CC2=C1NN=C2 GQKYKPLGNBXERW-UHFFFAOYSA-N 0.000 description 1
- 206010017577 Gait disturbance Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- CMJCEVKJYRZMIA-UHFFFAOYSA-M thallium(i) iodide Chemical compound [Tl]I CMJCEVKJYRZMIA-UHFFFAOYSA-M 0.000 description 1
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)
- Ceramic Products (AREA)
- Glass Compositions (AREA)
Description
産業上の利用分野
本発明は透光性アルミナセラミツクの封着材料
に関し、特にアルミナセラミツク管を用いたメタ
ルハライドランプの両端部に使用される封着用組
成物の改良に関する。
従来の技術
近年、メタルハライドランプは高い効率と演色
性の優れた実用的価値の高いランプとして照明の
各分野で多用されている。しかしながら、メタル
ハライドランプは、発光管材料として石英を用い
ているために高圧ナトリウムランプの発光管材料
として用いられているアルミナの様な耐熱性の高
いセラミツク等に比較して使用温度限界が低く、
ランプのより高い効率と演色性を得ようとした
時、この使用温度限界が障害になつていた。メタ
ルハライドランプにおいては発光管の管壁負荷を
高めるなどして動作温度を高めると、より高い効
率と演色性が得られるが、この様な高い温度には
石英が長時間耐えることができないために、ラン
プの短寿命をもたらす結果となつていた。
メタルハライドランプ動作中の発光管の最高温
度は発光管管体の中心部にあり、動作可能温度は
この部分の温度によつて規制され発光管端部の保
温板等の大きさによつて任意の蒸気圧が得られる
様に構成されている。そこでメタルハライドラン
プの動作温度を上げ、より高い効率と演色性を得
るために、石英製発光管に代えて、石英よりも耐
熱性と化学的安定性の高いアルミナセラミツク管
等を用いることが種々試みられている。
このセラミツク製発光管を用いたメタルハライ
ドランプにおいて、発光管端部の封着材料とし
て、例えばイギリス特許8010906号記載のSiO2−
Al2O3−MgO系封着材、特公昭49−32301号記載
のBeO−Al2O3−SiO2系封着材等が知られてい
る。これらの封着材を使用する際、まず発光管の
一端がシールされ、充填ガス及び添加物を封入し
た後、他端をシールするが、この他端のシール時
においてシールするための条件すなわち温度と時
間は添加物の揮発による損失あるいは充填ガスの
純度低下を最小限に抑えるように選定される。す
なわち、シール時の温度は比較的低温で、かつ短
時間でシールが完成されなければならないが、前
記の如き封着材組成中前者はシール時の急激な熱
衝撃とアルミナセラミツクとのわずかな膨張率の
違いにより、溶融固化後の封着材内部に微細なク
ラツクが多数発生し、発光管点灯と同時にこのク
ラツクが拡大されリークに至る例が多かつた。
又、後者の組成では封着時の溶融封着材の粘性が
高く、固化後セラミツクキヤツプとパイプとの間
の間隙が大となり、リークしやすくなつたり、粘
性が高いために気泡を取り込んだりして、シール
不良が発生しやすかつた。又、アルミナとの接着
強度に実用上の問題があつた。更に、このような
封着材は点灯中の高温のハロゲン蒸気に対する耐
ハロゲン性および封着作業の際の溶融温度を考慮
する必要がある。
発明が解決しようとする問題点
本発明は上記の点に鑑みなされたもので、セラ
ミツクとセラミツク又はセラミツクと金属とを封
着するための封着用組成物としてAl2O3、Y2O3、
La2O3、SiO2およびBeOを所定の組成比（重量
％）に選定することにより、耐ハロゲン性が高
く、溶融固化後の微細クラツク及び気泡の発生が
なく、かつ接着強度の高い封着材を得ることがで
き長寿命、高効率、高演色性を有するセラミツク
製メタルハライドランプを提供することを目的と
する。
問題点を解決するための手段
本発明者等はかかる封着材について多くの実験
を重ねた結果、Al2O3（酸化アルミニウム）、Y2O3
（酸化イツトリウム）、La2O3（酸化ランタン）、
SiO2（二酸化珪素）及びBeO（酸化ベリリウム）
のように耐ハロゲン性の高い成分を選定した。こ
こで、酸化ベリリウムは適量の添加によりアルミ
ナ基体との間に界面反応が生じ接着強度が大きく
溶融時粘性の低下が可能であることを見出し、良
好な封着材が得られることを確認した。
本発明は上記実験結果に基づいて完成されたも
のであり、その成分は次の含有組成をもつもので
ある。
Al2O3：５〜30重量％
Y2O3：10〜40重量％
La2O3：30〜70重量％
SiO2：５〜30重量％
BeO：２〜15重量％
作 用
上記の組成限定理由は、次の様なことに依る。
Al2O3量を30重量％以上とすると、封着材中に
気泡が多くなり結晶の析出が大となり、クラツク
が多発し、SiO2量を30重量％以上とすると、融
点降下が激しくなり、実用上問題となり、かつ熱
膨張率がAl2O3のそれよりも小さくなりすぎクラ
ツクが生じる。Y2O3量を40重量％以上とすると、
融点が1500℃以上となり、実用上問題となり、
BeO量を15重量％以上とすると、結晶性が大と
なりすぎ、気泡、クラツクが生じる。La2O3量を
70重量％以上とすると、気泡、クラツクが多発
し、リークしやすくなる。次に下限の限定理由を
述べると、SiO2、BeO、Al2O3、Y2O3量を限定
値以下とすると融点上昇が大となり実用上問題と
なりLa2O3を30重量％以下とすると、結晶の析出
が大きくなりすぎ結晶間にクラツクが多発しリー
クしやすくなる。
従つて、上記成分比内に各成分を調整すること
によつて、耐ハロゲン性が高く、アルミナセラミ
ツクとの熱膨張係数も許容限度内に合致し、更に
融点も1200〜1450℃以内の実用上全く問題のない
封着材が得られることがわかつた。
実施例
次に、本発明にかかる実施例を封着材の調合法
とともに述べる。
第１表に示す様な調合用原料を粉砕混合した
後、所望の形状に圧縮成形したものをセラミツク
管の端部とエンドキヤツプとの封着部に配置し、
同封着部を真空あるいは希ガス中で1400〜1600℃
に加熱することによつて同部を封着する。第１表
中の実施例No.１〜No.４において特性的に異なるの
は単に封着時における融点が多少異なることと、
結晶相とガラス相との比率が多少異なるのみであ
り、気泡はほとんどなく、クラツクもなく気密性
は良好であつた。
この様に前記実施例とさらに種々実験結果を組
合せると封着材組成として
Al2O3：５〜30重量％
Y2O3：10〜40重量％
La2O3：30〜70重量％
SiO2：５〜30重量％
BeO：２〜15重量％
の範囲からなる封着材であれば、十分満足すべき
封止状態が得られることが明らかとなつた。
この様に、管内に沃化タリウム、沃化デイスプ
ロシウムを各所定量封入した透光性アルミナセラ
ミツク発光管を用いたメタルハライドランプを作
成して、点灯試験を長時間行つたが、封止部のリ
ークは全く見られなかつた。
INDUSTRIAL APPLICATION FIELD The present invention relates to a sealing material for translucent alumina ceramic, and more particularly to an improvement in a sealing composition used at both ends of a metal halide lamp using an alumina ceramic tube. BACKGROUND OF THE INVENTION In recent years, metal halide lamps have been widely used in various lighting fields as lamps with high efficiency and excellent color rendering properties and high practical value. However, since metal halide lamps use quartz as the arc tube material, their operating temperature limit is lower than that of highly heat-resistant ceramics such as alumina, which are used as the arc tube material of high-pressure sodium lamps.
This operating temperature limit has been a stumbling block in efforts to achieve higher lamp efficiency and color rendering. In metal halide lamps, higher efficiency and color rendering can be obtained by increasing the operating temperature by increasing the wall load of the arc tube, but since quartz cannot withstand such high temperatures for long periods of time, This resulted in a shortened lamp life. The maximum temperature of the arc tube during operation of the metal halide lamp is at the center of the arc tube body, and the operating temperature is regulated by the temperature of this area, and can be adjusted to any desired temperature depending on the size of the heat insulating plate at the end of the arc tube. It is constructed to obtain vapor pressure. Therefore, in order to raise the operating temperature of metal halide lamps and obtain higher efficiency and color rendering, various attempts have been made to use alumina ceramic tubes, which have higher heat resistance and chemical stability than quartz, instead of quartz arc tubes. It is being In this metal halide lamp using a ceramic arc tube, for example, SiO 2 - described in British Patent No. 8010906 is used as a sealing material at the end of the arc tube.
Al2O3 - MgO-based sealing materials, BeO- Al2O3 - SiO2 - based sealing materials described in Japanese Patent Publication No. 49-32301, and the like are known. When using these sealing materials, one end of the arc tube is first sealed, the filler gas and additives are sealed, and then the other end is sealed, but the conditions for sealing, that is, the temperature, are required when sealing the other end. and time are selected to minimize losses due to volatilization of additives or loss of purity of the fill gas. In other words, the sealing temperature must be relatively low and the sealing must be completed in a short time; however, among the sealing material compositions mentioned above, the former is susceptible to rapid thermal shock during sealing and slight expansion with the alumina ceramic. Due to the difference in rate, many minute cracks were generated inside the sealing material after melting and solidification, and there were many cases in which these cracks enlarged at the same time as the arc tube was turned on, leading to leaks.
In addition, with the latter composition, the viscosity of the molten sealing material during sealing is high, and after solidification, the gap between the ceramic cap and the pipe becomes large, making it easy to leak, and the high viscosity causes air bubbles to be trapped. Therefore, seal failures were more likely to occur. In addition, there was a practical problem in the adhesive strength with alumina. Furthermore, it is necessary to consider the halogen resistance of such a sealing material to high-temperature halogen vapor during lighting and the melting temperature during sealing work. Problems to be Solved by the Invention The present invention has been made in view of the above points, and uses Al 2 O 3 , Y 2 O 3 ,
By selecting a predetermined composition ratio (wt%) of La 2 O 3 , SiO 2 and BeO, a seal with high halogen resistance, no minute cracks or bubbles after melting and solidification, and high adhesive strength can be achieved. The object of the present invention is to provide a metal halide lamp made of ceramic, which can be obtained from ceramic materials, has a long life, high efficiency, and high color rendering properties. Means for Solving the Problems As a result of many experiments with such sealing materials, the inventors found that Al 2 O 3 (aluminum oxide), Y 2 O 3
(yttrium oxide), La 2 O 3 (lanthanum oxide),
SiO 2 (silicon dioxide) and BeO (beryllium oxide)
We selected components with high halogen resistance. Here, it was discovered that by adding an appropriate amount of beryllium oxide, an interfacial reaction occurs between the beryllium oxide and the alumina substrate, resulting in high adhesive strength and a reduction in viscosity when melted, and it was confirmed that a good sealing material can be obtained. The present invention was completed based on the above experimental results, and its components have the following composition. Al 2 O 3 : 5-30% by weight Y 2 O 3 : 10-40% by weight La 2 O 3 : 30-70% by weight SiO 2 : 5-30% by weight BeO: 2-15% by weight Action Above composition The reason for the limitation is as follows. If the amount of Al 2 O 3 is more than 30% by weight, there will be many bubbles in the sealing material, crystal precipitation will be large, and cracks will occur frequently, and if the amount of SiO 2 is more than 30% by weight, the melting point will drop sharply. This is a practical problem, and the coefficient of thermal expansion becomes too small than that of Al 2 O 3 , causing cracks. When the amount of Y2O3 is 40% by weight or more,
The melting point is over 1500℃, which poses a practical problem.
When the amount of BeO is 15% by weight or more, the crystallinity becomes too large and bubbles and cracks occur. La 2 O 3 amount
If the content exceeds 70% by weight, bubbles and cracks will occur frequently and leaks will occur easily. Next, the reason for setting the lower limit is that if the amounts of SiO 2 , BeO, Al 2 O 3 , and Y 2 O 3 are below the limit values, the melting point will rise significantly, which is a practical problem, and La 2 O 3 must be kept at 30% by weight or less. As a result, the precipitation of crystals becomes too large and cracks occur frequently between the crystals, making it easy to leak. Therefore, by adjusting each component within the above-mentioned ratio, halogen resistance is high, the coefficient of thermal expansion with alumina ceramic is within the permissible limit, and the melting point is within the range of 1200 to 1450°C, which is practically impossible. It was found that a problem-free sealing material could be obtained. Examples Next, examples according to the present invention will be described together with a method of preparing a sealing material. After pulverizing and mixing the raw materials for preparation as shown in Table 1, the mixture is compression molded into a desired shape and placed in the sealing area between the end of the ceramic tube and the end cap.
The sealed part is heated to 1400 to 1600℃ in vacuum or rare gas.
The parts are sealed by heating to . The only difference in characteristics between Examples No. 1 to No. 4 in Table 1 is that the melting point at the time of sealing is slightly different.
There was only a slight difference in the ratio of the crystal phase to the glass phase, and there were almost no bubbles or cracks, and the airtightness was good. In this way, by combining the above examples and various experimental results, the composition of the sealing material is Al 2 O 3 : 5 to 30 weight % Y 2 O 3 : 10 to 40 weight % La 2 O 3 : 30 to 70 weight % It has become clear that a sealing material containing SiO2 : 5 to 30% by weight and BeO: 2 to 15% by weight can provide a sufficiently satisfactory sealing state. In this way, we created a metal halide lamp using a translucent alumina ceramic arc tube with predetermined amounts of thallium iodide and dysprosium iodide sealed inside the tube, and conducted lighting tests for a long time. No leaks were observed.
【表】【table】
【表】
発明の効果
以上の説明から明らかなように、本発明に係る
封着用組成物はセラミツクとセラミツク又はセラ
ミツクと金属とを封着した際、封着材内部に微細
なクラツクおよび気泡が生じることがなく、接着
強度も高く更に耐ハロゲン性に優れているのでリ
ークによるランプの不点事故を防止することがで
きる。
又、封着材の融点を適切な範囲に選定できるの
で、作業性が良い等の利点を有する。[Table] Effects of the Invention As is clear from the above description, when the sealing composition of the present invention seals ceramic to ceramic or ceramic to metal, fine cracks and bubbles are generated inside the sealing material. It has high adhesive strength and excellent halogen resistance, so it can prevent lamp malfunctions due to leakage. Further, since the melting point of the sealing material can be selected within an appropriate range, there are advantages such as good workability.
Claims (1)
Y2O3、30〜70重量％のLa2O3、５〜30重量％の
SiO2及び２〜15重量％のBeOを含有してなるセ
ラミツクとセラミツク又はセラミツクと金属とを
封着するための封着用組成物。1 5-30% by weight Al 2 O 3 , 10-40% by weight
Y 2 O 3 , 30-70% by weight La 2 O 3 , 5-30% by weight
A sealing composition for sealing ceramic and ceramic or ceramic and metal, which contains SiO 2 and 2 to 15% by weight of BeO.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13006484A JPS6110082A (en) | 1984-06-26 | 1984-06-26 | Sealing composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13006484A JPS6110082A (en) | 1984-06-26 | 1984-06-26 | Sealing composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6110082A JPS6110082A (en) | 1986-01-17 |
| JPH0411511B2 true JPH0411511B2 (en) | 1992-02-28 |
Family
ID=15025150
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13006484A Granted JPS6110082A (en) | 1984-06-26 | 1984-06-26 | Sealing composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6110082A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006106781A1 (en) * | 2005-03-31 | 2006-10-12 | Nippon Sheet Glass Company, Limited | Glass composition containing yttrium and glass spacer for electron beam excitation type display |
| DE102010012524B4 (en) * | 2010-03-19 | 2012-03-15 | Schott Ag | Glass ceramic as a dielectric in the high frequency range, process for the preparation and use of such |
-
1984
- 1984-06-26 JP JP13006484A patent/JPS6110082A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6110082A (en) | 1986-01-17 |
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