JPS5869749A - Quartz glass sealed product - Google Patents
Quartz glass sealed productInfo
- Publication number
- JPS5869749A JPS5869749A JP16777181A JP16777181A JPS5869749A JP S5869749 A JPS5869749 A JP S5869749A JP 16777181 A JP16777181 A JP 16777181A JP 16777181 A JP16777181 A JP 16777181A JP S5869749 A JPS5869749 A JP S5869749A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- quartz glass
- melting point
- low melting
- sealant
- 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.)
- Granted
Links
Abstract
Description
【発明の詳細な説明】
固に接着し気密性に優れた石英ガラス封着体に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a quartz glass sealed body that is firmly adhered and has excellent airtightness.
昨今、光フアイバーケーブルのコネクターとして利用す
るために石英ガラスとコパール金具との封着について種
々試みられているが、要求されるＩｆＩ性が両者を強固
に接着し、ハーメチックシール的に接着する必要上、そ
の問題点は解決するに至っていない。このハーメチック
シール的に接着させるためには、両者の熱膨張係数の差
が小さいことが必要条件であるが、石英ガラスとコパー
ル金具の熱膨張係数は、それぞれｊ ｘ １０−’ Ｃ
−” 、 ０１ ｘ ／（ｒ’℃−１であ）、：ｓパ−
ｈ金具が石英ガラスに比べ２倍と大きい．この２倍の熱
膨張差がある材料同志を接着するＯは従来の一般的考え
では不可能とされていた．そのため、本研究者社石英ガ
ラスとコパール金具との間に中間層を設けて接着する方
法を試み、どんな材料でどのぐらいの熱膨張係数のもの
がよいか検討された．材料としては石英ガラスとコパー
ル金具とに最も適合し九ガラスを選択し、そのガラスも
石英ガラスの常用安全使用温度７０００℃の耐熱性を考
慮して低融点ガラスにて検討された、また、熱膨張係数
は石英ガラスとコパール金具との中間％膨張係数が妥当
であるとの見解と、その熱膨張係数に併せて接着強度も
向上させる添加物の研究を鋭意努力した結果、石英ガラ
スとコパール金具とを強固に接着し、かつ気密性に優れ
た封着体を完成しえ。Recently, various attempts have been made to seal quartz glass and copal metal fittings for use as optical fiber cable connectors, but the required IfI properties require a strong bond between the two and a hermetic seal. , the problem has not yet been resolved. In order to achieve this hermetic sealing, it is necessary that the difference in thermal expansion coefficients between the two be small, and the thermal expansion coefficients of quartz glass and copal metal fittings are j x 10-'C, respectively.
−”, 01 x/(at r'℃−1), :s par-
The H metal fittings are twice as large as those of quartz glass. Conventional general thinking had it that it was impossible to bond materials with twice this difference in thermal expansion. Therefore, the researchers tried a method of bonding by creating an intermediate layer between the quartz glass and the copal metal fittings, and examined what kind of material and what coefficient of thermal expansion would be best. As for the material, 9 glass was selected as it is most compatible with the quartz glass and copal metal fittings. As a result of the idea that the expansion coefficient is appropriate to be the intermediate % expansion coefficient between quartz glass and copal metal fittings, and as a result of diligent research into additives that improve the adhesive strength as well as the thermal expansion coefficient, quartz glass and copal metal fittings A sealed body with excellent airtightness and strong adhesion can be created.
本発明の要旨は、石英ガラスとコパール金具との間に低
融点ガラスを介在して加熱処理し封着することを特徴と
するものであシ、これに使用する低融点ガラスは、市販
の低融点系ガラスにガラス強化剤としてホワイトアラン
ダムＷＡΦｔｏｏｏ １１− ｉｏ −ｕｏ重量９６を
加えたもので、この低融点ガラスは熱膨張係数が３０〜
コ！θ℃のときａ＝コ０−４１０ｘ１０−’℃−１のも
のである。The gist of the present invention is characterized in that a low melting point glass is interposed between the quartz glass and the copal metal fittings, and the low melting point glass used for this is a commercially available low melting point glass. It is made by adding White Alundum WAΦtoo 11-io-uo weight 96 as a glass strengthening agent to melting point glass, and this low melting point glass has a thermal expansion coefficient of 30~
Ko! When θ°C, a=ko0-410x10-'°C-1.
上記、ＷＡφ１ｏｏｏ ｔｔｏ−参〇重量−の範囲内で
加えた理由は、その範囲内では石英ガラスとコパール金
具との封着されたガラス表面は、肉眼の観察では亀裂の
発生も殆んどなく良好であり、その接着強度は２３０〜
Ｉ１０’１４であって、気密性も／ ｘ ／ Ｏ’ｃｃ
／ｓｅｅの値があシ実用性の高いものであった。しかし
、１０重量−以下では封着されたガラス表面に小さな亀
裂の発生が認められ、接着強度は３０−／１０１１であ
り、気密性は０〜／ ｘ ／ ０−ｓであつえ、まえ、
＃０重量−以上で嬬、焼結温度が高（な〕、封着された
ガラス表面はガサガサの状態で接着強度はｔｏ６以下で
あシ、気密性は／ｘ／（１”であった。The reason for adding the above weight within the range of WAφ1oootto is that within that range, the sealed glass surface of the quartz glass and copal metal fittings is in good condition with almost no cracks when observed with the naked eye. The adhesive strength is 230~
I10'14 and airtight / x / O'cc
The value of /see was highly practical. However, if the weight is less than 10, small cracks are observed on the sealed glass surface, the adhesive strength is 30/1011, and the airtightness is 0~/x/0-s.
#0 weight or more, the sintering temperature was high, the sealed glass surface was rough, the adhesive strength was less than to6, and the airtightness was /x/(1'').
また、低融点ガラスの熱膨張係＄ｔＪＯ〜２１０℃のと
き−−Ｊ０〜４！Ｏｘ １０−’ｒ”Ｋ＠定した理由は
、フィラーとしてＷムす１０００を加えるとｄは大きく
なり、コパールの−よ〕大きくなシ、封着体としてのガ
ラスに引張ル応力がかか）、気密性が保たれないためで
ある。Also, when the thermal expansion coefficient of low melting point glass is $tJO~210°C--J0~4! The reason for determining Ox 10-'r"K@ is that when 1000 W is added as a filler, d increases, and as with copal, tensile stress is applied to the glass as a sealing body. This is because airtightness cannot be maintained.
以下、実施例により詳細に説明する。Hereinafter, it will be explained in detail using examples.
実施例
ここでの低融点ガラスとは、Ｐｂｏ −Ｂ２０ａ −Ｚ
ｎＯ系にＰｂＴｉＯｓまたはＺｒ８１０４或いはツーデ
ィ２イト （λＭｇＯ・ＪＡｂＯｓ −７８１０ｍ ）
勢を少量、フィラーとして含有しているものを指す。Examples The low melting point glass here is Pbo-B20a-Z
PbTiOs or Zr8104 or two diite (λMgO・JAbOs -7810m) in nO system
It refers to a product that contains a small amount of filler as a filler.
市販品の低融点ガラスにフィラーとしてＷＡφ１０００
を下記ＩＩ１表の割合でアルよす製ボットミル中でアル
ミナ球石を使用して混合した。WAφ1000 as a filler in commercially available low melting point glass
were mixed using an alumina coccule in a bot mill manufactured by Alyosu in the proportions shown in Table II1 below.
／
／′
／
／
／
／′
７／
この混合粉末を使用して、ＮＴＫマイカセラミックス製
の皺にて円筒状直参−×１２−×まコＬ■をプレス成形
し、２００℃で仮焼してプリフォームとした。／ ／' ／ ／ ／ ／' 7/ Using this mixed powder, press mold a cylindrical straight-x12- It was made into a preform.
次に石英ガラス棒１０ｆｘｌＯＬ■に上記プリフォ一本
を挿入し、その外側にマパールリングｉｏ、ｚφ×４．
ｊφｘｊＬ■をセットして、第一図の断向図に示す如く
カーボン治具ｌ参にセットしてシールガラス封着温［１
００℃で／ｊ分間引延して接着した０図中ｉｉは石英ガ
ラス棒で厚さＱ４鱈のシールガラスプリ７オーム１３を
挿入し）その外側にコバールリング／コをセットしたも
のである。その完成品を第１図の断面図に示し封着ガラ
スＪの厚み０．７７ｍを得た。Next, insert one of the above-mentioned prefo into the quartz glass rod 10fxlOL■, and put Mapal ring io, zφ×4.
jφ
In Figure 0, ii is a quartz glass rod with a Q4 thickness sealing glass pre-7 ohm 13 inserted and a Kovar ring set on the outside. The completed product is shown in the sectional view of FIG. 1, and a sealing glass J having a thickness of 0.77 m was obtained.
これらの試料を引張り試験機である高滓オートグラフ５
４００を使用して接着強度を測定しまた気缶性について
は、ＨｅリークディテクターＶｅｅｃｏ ＭＥＪ／Ｉに
て測定し下記嬉コ表に示した。These samples were tested using a tensile tester, Takashi Autograph 5.
400 was used to measure the adhesive strength, and the air resistance was measured using a He leak detector Veeco MEJ/I, and the results are shown in the table below.
上記、試料の測定値は各３個の平均値を示したもので、
本発明である市販のＰｂ０−ＢｘＯｓ −ＺｎＯ系ガラ
スにＷＡφ１ｏｏｏ ｔｉｏ〜ｓｏ重量−を加えた封着
体試料の１３〜ｔのものは、外観、接着強度、気密性と
も良好なものであつ九。The above measurement values for the samples are the average values of each three samples.
The sealing body samples of the present invention, which are commercially available Pb0-BxOs-ZnO glass and WAφ1ooo tio-so weight- were added, had good appearance, adhesive strength, and airtightness.
以上の実施例で記述し九低融点ガラスは、ＰｂＯ−Ｂｘ
Ｏｓ −ＺｎＯ系についてであるが、其の他のＰｂＯ−
ＢｘＯｓ −８１０ａ系やＰｂＯ−ＢｚＯｓ −Ａ１１
ｏｓ系にＷムす１ｏｏｏ ｔ−１ｏ−、、＃ｏ重量−加
えたものでも、同等差違ない良好な結果を得ることが出
来た。The nine low melting point glasses described in the above examples are PbO-Bx
Regarding the Os-ZnO system, other PbO-
BxOs-810a series and PbO-BzOs-A11
Similar good results could be obtained even when W weight was added to the os system.
本発明の石英ガラス封着体は、原子力用ペネトレーシ曹
ンや光７アイパー撮像管コネクターとして使用出来る産
業上値れたものである。The quartz glass sealed body of the present invention is industrially valuable and can be used as a nuclear power penetration chamber or an optical 7-eyeper image pickup tube connector.
第７図は石英ガラスに：１パール金具會封着した断面図
、第２図は熱処理前の治具にセットした断面図である。
１、ｌノ・・・石英ガラス、コ、／Ｊ・・・コバール金
具、３・・・封着体、１３・・・封着仮焼体、１４Ｉ・
・・カーボン治具
第１図
第２図FIG. 7 is a sectional view of the quartz glass sealed with a pearl metal fitting, and FIG. 2 is a sectional view of the quartz glass set in a jig before heat treatment. 1, L... quartz glass, /J... Kovar metal fittings, 3... sealed body, 13... sealed calcined body, 14 I...
・・Carbon jig Fig. 1 Fig. 2
Claims (1)
ラスを介在して加熱処理し封着することを特徴とする石
英ガラス封着体。 Ｑ）特許請求の範１８Ｉ＃Ｉ／項記載の低融点ガラスは
、市販の低融点系ガラスにガラス強化剤としてホワイト
アランダムＷムφ１ｏｏｏｔ−ｉｏ〜参Ｏ重量％を加え
たものであることｔ−特徴とする石英ガラス封着体。 （３）％許請求の範囲第７項ま九は第２項記載の低融点
ガラスは熱膨張係数が３０−コｊ０℃のときα−ココ０
〜＃０ｘ１０’１であることｔ−特徴とする石英ガラス
封着体。[Scope of Claims] (1) A quartz glass sealed body characterized by interposing a low melting point glass between quartz glass and copal metal fittings and sealing them by heat treatment. Q) The low melting point glass described in claim 18I#I/ is a commercially available low melting point glass to which white alundum W φ1ooot-io ~ 0% by weight is added as a glass strengthening agent. -Characteristic quartz glass sealed body. (3) Permissible %Claims 7 and 9 indicate that the low melting point glass described in paragraph 2 has a coefficient of thermal expansion of 30 - 0 at 0°C.
A quartz glass sealed body characterized by being ~#0x10'1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16777181A JPS5869749A (en) | 1981-10-20 | 1981-10-20 | Quartz glass sealed product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16777181A JPS5869749A (en) | 1981-10-20 | 1981-10-20 | Quartz glass sealed product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5869749A true JPS5869749A (en) | 1983-04-26 |
| JPH0222014B2 JPH0222014B2 (en) | 1990-05-17 |
Family
ID=15855791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16777181A Granted JPS5869749A (en) | 1981-10-20 | 1981-10-20 | Quartz glass sealed product |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5869749A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6389438A (en) * | 1986-09-30 | 1988-04-20 | Nippon Sheet Glass Co Ltd | Bonding structure between glass and metal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5455019A (en) * | 1977-10-11 | 1979-05-01 | Tokyo Shibaura Electric Co | Method of making window member |
-
1981
- 1981-10-20 JP JP16777181A patent/JPS5869749A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5455019A (en) * | 1977-10-11 | 1979-05-01 | Tokyo Shibaura Electric Co | Method of making window member |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6389438A (en) * | 1986-09-30 | 1988-04-20 | Nippon Sheet Glass Co Ltd | Bonding structure between glass and metal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0222014B2 (en) | 1990-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3676292A (en) | Composites of glass-ceramic-to-metal,seals and method of making same | |
| US4678868A (en) | Hermetic electrical feedthrough assembly | |
| US3726987A (en) | Glass or ceramic-to-metal seals | |
| GB822272A (en) | Composite article and method of joining preformed parts to form such article | |
| US3120433A (en) | Method of joining glass components by radiant energy | |
| US3414465A (en) | Sealed glass article of manufacture | |
| KR20160058859A (en) | Silicic acid mixtures and use thereof as insulation material | |
| US2389386A (en) | Glazed ceramic | |
| US2098812A (en) | Ceramic material | |
| EP0029275B1 (en) | Bodies composed of at least two parts, sealing glass and method for bonding parts | |
| US4537863A (en) | Low temperature sealing composition | |
| JPS5869749A (en) | Quartz glass sealed product | |
| KR100573550B1 (en) | Sealing composition | |
| CN107218958A (en) | A kind of measuring electrode and preparation method thereof | |
| SU1437360A1 (en) | Method of joining sapphire to metal | |
| SU1456390A1 (en) | Glass solder for soldering tungsten with ceramic materials | |
| JPH0539476A (en) | Sealing material | |
| JPH01226749A (en) | Glass composition for joining ceramic | |
| JPS6158835A (en) | Enamel glaze composition | |
| CN101759367B (en) | Al2O3-Dy2O3-SiO2 ternary system rare-earth sealing material and preparation method of glass sealing ring thereof | |
| JPH0217938B2 (en) | ||
| JPH06331594A (en) | Method for sealing cell part of oxygen sensor | |
| JPH0640456B2 (en) | Bonded porcelain insulator | |
| JPS63162584A (en) | Joined body of silicon nitride base sintered body and joining method | |
| SU1765142A1 (en) | Method of connecting articles made of vacuum-compact ceramics |