JPH0376024B2 - - Google Patents
Info
- Publication number
- JPH0376024B2 JPH0376024B2 JP14187786A JP14187786A JPH0376024B2 JP H0376024 B2 JPH0376024 B2 JP H0376024B2 JP 14187786 A JP14187786 A JP 14187786A JP 14187786 A JP14187786 A JP 14187786A JP H0376024 B2 JPH0376024 B2 JP H0376024B2
- Authority
- JP
- Japan
- Prior art keywords
- metal shell
- cap
- plating
- melting point
- low melting
- 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
- 229910052751 metal Inorganic materials 0.000 claims description 72
- 239000002184 metal Substances 0.000 claims description 72
- 239000011521 glass Substances 0.000 claims description 56
- 238000007747 plating Methods 0.000 claims description 53
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 34
- 238000002844 melting Methods 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 23
- 230000003287 optical effect Effects 0.000 claims description 8
- 238000005554 pickling Methods 0.000 claims description 8
- 239000003929 acidic solution Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 32
- 229910052759 nickel Inorganic materials 0.000 description 16
- 238000000034 method Methods 0.000 description 11
- 239000007795 chemical reaction product Substances 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 229910000833 kovar Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001444 catalytic combustion detection Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
- Joining Of Glass To Other Materials (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、レーザダイオード、CCDなどの光
素子用キヤツプの製造方法に関し、詳しくはガラ
ス封着された光素子用キヤツプの仕上げメツキ及
びその前処理工程の改良に関する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for manufacturing caps for optical devices such as laser diodes and CCDs, and more specifically, finishing plating and pretreatment steps for glass-sealed caps for optical devices. Regarding the improvement of
従来の技術
光素子用キヤツプは、矩形や円形の窓孔を有す
る金属シエルの窓孔周辺部に、透孔性ガラス板を
低融点ガラスで気密に接着固定した構造が一般的
で、その一例を第３図及び第４図を参照して説明
する。Conventional technology Caps for optical devices generally have a structure in which a permeable glass plate is hermetically bonded and fixed with low melting point glass around the window hole of a metal shell having a rectangular or circular window hole. This will be explained with reference to FIGS. 3 and 4.
第３図は光素子用キヤツプ１の平面図、第４図
は第３図のＡ−Ａ線に沿う断面図で、同図におい
て、２は矩形のコバール〔Fe−Ni−Co合金〕製
の金属シエルで、矩形の天板部２ａと、天板部２
ａの４辺より下方に絞り加工された筒部２ｂと、
筒部２ｂの下端より外方に延びるフランジ部２ｃ
から成り、天板部２ａの中央部に矩形の窓孔３が
形成される。４は金属シエル２の窓孔３を塞ぐ矩
形の透光性ガラス板で、コバール製金属シエル２
と同様な熱膨張係数のホウケイ酸ガラスの板であ
る。５は金属シエル２の天板部２ａと筒部２ｂの
コーナ部分内側にガラス板４を気密に接着固定す
る低融点ガラスで、酸化鉛を主成分とする。 FIG. 3 is a plan view of the optical device cap 1, and FIG. 4 is a sectional view taken along line A-A in FIG. A metal shell with a rectangular top plate part 2a and a top plate part 2
a cylindrical portion 2b drawn downward from the four sides of a;
Flange portion 2c extending outward from the lower end of the cylindrical portion 2b
A rectangular window hole 3 is formed in the center of the top plate portion 2a. 4 is a rectangular translucent glass plate that closes the window hole 3 of the metal shell 2;
It is a plate of borosilicate glass with a coefficient of thermal expansion similar to that of . Reference numeral 5 denotes a low melting point glass, which is used to airtightly adhere and fix the glass plate 4 to the inside of the corner portions of the top plate portion 2a and the cylindrical portion 2b of the metal shell 2, and contains lead oxide as a main component.
このようなキヤツプ１の製造は、通常は次のガ
ラス封着工程、酸洗い工程、光沢洗い工程、表面
洗浄工程、無電解ニツケルメツキによる仕上げメ
ツキ工程で行われる。 The manufacture of such a cap 1 is normally carried out through the following glass sealing process, pickling process, brightening process, surface cleaning process, and finish plating process using electroless nickel plating.
先ず、コバール製金属シエル２の全表面に低融
点ガラス５とのなじみ性の良い酸化膜を形成して
おいて、金属シエル２にガラス板４を低融点ガラ
ス５で接着固定する〔ガラス封着工程〕。尚、金
属シエル２の表面に酸化膜を形成せず、コバール
の素地上に低融点ガラス５を溶着させると、コバ
ール素地はガラスとのなじみ性が悪くて、金属シ
エル２と低融点ガラス５間の気密性が悪くなる。 First, an oxide film that is compatible with the low melting point glass 5 is formed on the entire surface of the metal shell 2 made of Kovar, and the glass plate 4 is adhesively fixed to the metal shell 2 with the low melting point glass 5 [Glass sealing] process]. Note that when the low melting point glass 5 is welded onto the Kovar base without forming an oxide film on the surface of the metal shell 2, the Kovar base has poor compatibility with the glass, and the gap between the metal shell 2 and the low melting point glass 5 increases. airtightness deteriorates.
次に、ガラス封着されたキヤツプ１の金属シエ
ル２の露出表面に防錆等の目的で仕上げメツキす
るために、その前処理として、先ず金属シエル２
の露出した表面上の酸化膜を除去する酸洗いを行
なう。これはキヤツプ１を10〜30％濃度の塩酸溶
液に浸漬して、金属シエル２の表面の酸化膜を塩
酸HClで溶かすことで行われる。 Next, in order to finish plating the exposed surface of the metal shell 2 of the glass-sealed cap 1 for purposes such as rust prevention, the metal shell 2 is first treated as a pretreatment.
A pickling process is performed to remove the oxide film on the exposed surface. This is done by immersing the cap 1 in a 10-30% hydrochloric acid solution and dissolving the oxide film on the surface of the metal shell 2 with the hydrochloric acid HCl.
このように塩酸で酸洗いされたキヤツプ１の金
属シエル２表面は凹凸面になつているので、この
凹凸面を円滑面にして後の仕上げメツキを良好に
するため、先ずキヤツプ１を濃硫酸が96vol％で
残りが濃硝酸である混合溶液に浸漬して、金属シ
エル２の表面を予備洗いしてから、次にキヤツプ
１を酢酸溶液84vol％と、濃硝酸溶液13vol％と、
塩酸溶液の混合溶液1vol％に浸漬して、金属シエ
ル２の表面を光沢のある円滑面にする。次に、光
沢洗いされたキヤツプ１の金属シエル２表面は水
との親和性に劣り、後の仕上げメツキのメツキ液
を弾き易いので、キヤツプ１の金属シエル２表面
を９％濃度の塩酸溶液で洗浄して、金属シエル２
の表面の水との親和性を良好にしておく〔表面洗
浄〕。 The surface of the metal shell 2 of the cap 1 that has been pickled with hydrochloric acid has an uneven surface, so in order to make the uneven surface a smooth surface for better finish plating, the cap 1 was first washed with concentrated sulfuric acid. After pre-washing the surface of metal shell 2 by immersing it in a mixed solution of 96 vol% and the rest being concentrated nitric acid, cap 1 was soaked in 84 vol% acetic acid solution and 13 vol% concentrated nitric acid solution.
The metal shell 2 is immersed in a 1 vol% mixed solution of hydrochloric acid to make the surface of the metal shell 2 shiny and smooth. Next, the surface of the metal shell 2 of the cap 1 that has been polished has poor affinity with water and easily repels the plating solution used in the final plating, so the surface of the metal shell 2 of the cap 1 is coated with a 9% hydrochloric acid solution. Clean and metal shell 2
Maintain good affinity with water on the surface [Surface cleaning].
最後に、上述のように前処理されたキヤツプ１
を無電解ニツケルメツキ液に浸漬して、キヤツプ
１の金属シエル２の表面にメツキ液中のニツケル
を化学的に還元させて付着させ、金属シエル２の
表面に無電解ニツケルメツキ層を形成する〔仕上
げメツキ〕。 Finally, cap 1 is pretreated as described above.
is immersed in an electroless nickel plating solution, and the nickel in the plating solution is chemically reduced and adhered to the surface of the metal shell 2 of the cap 1, thereby forming an electroless nickel plating layer on the surface of the metal shell 2. ].
発明が解決しようとする問題点
ところが、上記キヤツプ１の製造においては、
仕上メツキが良好に行えない問題がある。即ち、
ガラス封着が完了したキヤツプ１を10〜30％濃度
の塩酸溶液で酸洗いし、また、光沢洗いした後、
９％濃度の塩酸溶液で表面洗浄しているが、低融
点ガラス５は硫酸系に強いが塩酸系に弱い物性が
あつて、上記の２回の塩酸溶液へのキヤツプ１の
浸漬時に、低融点ガラス５に含まれる鉛成分が塩
酸と化学反応して、その反応生成物が低融点ガラ
ス５の露出表面から外に溶出していく。また、キ
ヤツプ１を無電解ニツケルメツキ液に浸漬して仕
上げメツキを施す際に、メツキ液の酸と低融点ガ
ラス５の鉛成分が反応して、その反応生成物が低
融点ガラス５の露出表面から溶出する。このよう
な低融点ガラス５の表面から溶出する鉛成分の反
応生成物の多くは、塩酸溶液やメツキ液中に溶出
してキヤツプ１から離れるが、一部は低融点ガラ
ス５の表面から金属シエル２の表面に沿つて流れ
て、金属シエル２の表面に付着したり、メツキ時
においては金属シエル２の表面を部分的に覆うこ
とがある。そのため、キヤツプ１を仕上げメツキ
すると、金属シエル２の表面の上述反応生成物が
在る部分でのメツキ速度が他より遅れたり、メツ
キができなくなることがあつて、金属シエル２の
表面を均一に仕上げメツキすることが難しく、ま
た、金属シエル２の表面のメツキ面に光沢の斑が
生じて、キヤツプ１の品質や外観が悪くなること
があつた。Problems to be Solved by the Invention However, in manufacturing the above cap 1,
There is a problem that the finish plating cannot be performed well. That is,
After the glass sealing has been completed, cap 1 is pickled with a 10-30% hydrochloric acid solution, and after being polished,
Although the surface was cleaned with a 9% concentration hydrochloric acid solution, the low melting point glass 5 has physical properties that are strong against sulfuric acid systems but weak against hydrochloric acid systems. The lead component contained in the glass 5 chemically reacts with hydrochloric acid, and the reaction product is eluted out from the exposed surface of the low melting point glass 5. Furthermore, when the cap 1 is immersed in an electroless nickel plating solution for finishing plating, the acid in the plating solution reacts with the lead component of the low melting point glass 5, and the reaction product is released from the exposed surface of the low melting point glass 5. Elute. Most of the reaction products of the lead component eluted from the surface of the low melting point glass 5 are eluted into the hydrochloric acid solution or the plating solution and leave the cap 1, but some of them are leached from the surface of the low melting point glass 5 into the metal shell. It may flow along the surface of the metal shell 2 and adhere to the surface of the metal shell 2, or it may partially cover the surface of the metal shell 2 during plating. Therefore, when finish plating the cap 1, the plating speed on the surface of the metal shell 2 where the above-mentioned reaction products are present may be slower than other parts, or plating may not be possible, so that the surface of the metal shell 2 may not be uniform. Finish plating is difficult, and the plating surface of the metal shell 2 has uneven gloss, which sometimes deteriorates the quality and appearance of the cap 1.
そこで、上記問題のため、最近は上記キヤツプ
１の製造を次のように行つている。先ず、金属シ
エル２にガラス板４を固定する前に、金属シエル
２の全表面を酸洗い、光沢洗いしてから仕上げメ
ツキを施しておく。而して、この金属シエル２に
ガラス板４を低融点ガラス５で接着固定する。こ
のようにすれば常に良好な仕上げメツキが施され
たキヤツプ１が得られる。しかし、ガラス封着前
に仕上げメツキされた金属シエル２の表面のメツ
キ層はガラスとのなじみ性が悪く、そのため、金
属シエル２への低融点ガラス５の付着力が弱く
て、この両者間で気密洩れが生じる可能性が大で
ある問題があつた。 In view of the above problem, the cap 1 has recently been manufactured as follows. First, before fixing the glass plate 4 to the metal shell 2, the entire surface of the metal shell 2 is pickled, polished, and then finished with plating. Then, a glass plate 4 is adhesively fixed to this metal shell 2 with a low melting point glass 5. In this way, a cap 1 with good finish plating can always be obtained. However, the plating layer on the surface of the metal shell 2, which has been finish plated before glass sealing, has poor compatibility with the glass, and therefore the adhesion of the low melting point glass 5 to the metal shell 2 is weak, and the bond between the two is poor. There was a problem where there was a high possibility of airtight leakage.
そこで、金属シエル２の低融点ガラス５でガラ
ス板４を接着固定する部分をマスク材でカバーし
て、ニツケルメツキ等のメツキをした後に、マス
ク材を除去し予備酸化して、ガラス板４を接着固
定するか、或は予備酸化した金属シエル２の低融
点ガラス５でガラス板４を接着固定する部分をマ
スク材でカバーしてニツケル等のメツキを施して
から、マスク材を除去して、ガラス板４を接着固
定することも提案されている〔特開昭58−46657
号公報〕。 Therefore, after covering the part of the metal shell 2 where the glass plate 4 is bonded and fixed with the low melting point glass 5 with a masking material and plating with nickel plating or the like, the masking material is removed and pre-oxidized, and the glass plate 4 is bonded. The part where the glass plate 4 is to be fixed or fixed with the low melting point glass 5 of the pre-oxidized metal shell 2 is covered with a mask material and plated with nickel or the like, and then the mask material is removed and the glass plate 4 is fixed. It has also been proposed to fix the plate 4 with adhesive [JP-A-58-46657
No. Publication].
しかしながら、このように個々の金属シエル２
に部分的にマスク材を被着することは非常に煩雑
であり、特に金属シエル２の天板部２ａと筒部２
ｂの内面コーナ部に正確に被着することは困難
で、光素子用キヤツプが著しく高価なものになる
という問題点があつた。 However, in this way the individual metal shells 2
It is very complicated to partially apply mask material to the metal shell 2, especially the top plate part 2a and the cylinder part 2 of the metal shell 2.
It is difficult to accurately attach the cap to the inner corner portion of the optical element, and there is a problem in that the cap for the optical device becomes extremely expensive.
問題点を解決するための手段
本発明は上記問題点に鑑みて提案されたもの
で、金属シエルにガラス板を低融点ガラスで接着
固定したキヤツプにおける金属シエル表面への仕
上げメツキを良好に行うことを目的とし、この目
的を、前記キヤツプを塩酸を除く、硫酸を主体と
する酸性溶液で酸洗いすること、及び酸洗いされ
たキヤツプを無電解金属メツキ液に浸漬し、キヤ
ツプの金属シエルに電圧を印加して金属シエル表
面を仕上げメツキすることで達成するようにした
ものである。Means for Solving the Problems The present invention has been proposed in view of the above problems, and it is an object of the present invention to satisfactorily finish plating the surface of the metal shell in a cap in which a glass plate is adhesively fixed to the metal shell with low melting point glass. For this purpose, the cap is pickled with an acidic solution mainly composed of sulfuric acid excluding hydrochloric acid, and the pickled cap is immersed in an electroless metal plating solution, and a voltage is applied to the metal shell of the cap. This is achieved by applying a 100% irradiation temperature to finish plating the surface of the metal shell.
作 用
キヤツプを硫酸を主体とする溶液で酸洗いした
場合、キヤツプの金属シエルにガラス板を固定す
る低融点ガラスは硫酸系溶液に対して化学的に反
応し難くて、酸洗い時の低融点ガラスの溶出はほ
とんど無くなる。また、キヤツプの金属シエルに
電圧を印加して無電解金属メツキを施すと、低融
点ガラスがメツキ液中に溶出する前に、金属シエ
ル表面への無電解金属メツキが始まる。以上の２
つの作用にて、キヤツプの金属シエル表面への仕
上げメツキが均一に、良質に実行される。Effect When the cap is pickled with a solution containing mainly sulfuric acid, the low melting point glass that fixes the glass plate to the metal shell of the cap is chemically difficult to react with the sulfuric acid solution, so the low melting point during pickling is Glass elution is almost eliminated. Further, when electroless metal plating is performed by applying a voltage to the metal shell of the cap, electroless metal plating on the surface of the metal shell starts before the low melting point glass is eluted into the plating solution. Above 2
Through these two actions, the finish plating on the surface of the metal shell of the cap is performed uniformly and with good quality.
実施例
以下、本発明方法の具体的実施例を、第３図及
び第４図のキヤツプ１の製造において、第１図及
び第２図を参照して説明する。EXAMPLE A specific example of the method of the present invention will be described below with reference to FIGS. 1 and 2 in the manufacture of the cap 1 shown in FIGS. 3 and 4.
先ず、コバール製の金属シエル２の全表面に酸
化膜を形成して、この金属シエル２にガラス板４
を低融点ガラス５で接着固定したキヤツプ１を得
る。 First, an oxide film is formed on the entire surface of a metal shell 2 made of Kovar, and a glass plate 4 is attached to this metal shell 2.
A cap 1 is obtained by adhering and fixing with a low melting point glass 5.
次にキヤツプ１に防錆等の目的で行われる仕上
げメツキの前処理として、先ずキヤツプ１を酸洗
いする。この酸洗いを本発明は、塩酸を除く、硫
酸を主体とする酸性溶液に浸漬して行う。具体的
には、第１図に示すように、槽６内に濃硫酸が90
〜98vol％で残りが濃硝酸の酸性溶液７を収容し
て、この酸性溶液７にキヤツプ１を浸漬する。ま
た、槽６の一部に超音波発振原８を取付けて、酸
性溶液７に超音波振動を付与しておく。すると、
酸性溶液７中でキヤツプ１の金属シエル２の露出
表面の酸化膜の下地のコバール素地が硫酸
H2SO4と硝酸HNO2に侵蝕されて、酸化膜がその
下地から剥れ、これに超音波振動が加わつて酸化
膜は金属シエル２の表面から剥離除去される。こ
のような酸化膜除去を目的とした酸洗いにおい
て、キヤツプ１の低融点ガラス５は硫酸や硝酸に
対して化学的に強く、従つて、低融点ガラス５の
鉛成分の溶出現象はほとんど起らない。尚、上記
酸洗い時に超音波波振動を加えることは必ずしも
必要でないが、超音波振動を加えることで金属シ
エル表面の酸化膜剥離が確実、高速に行える。 Next, as a pretreatment for finish plating performed on the cap 1 for the purpose of rust prevention, etc., the cap 1 is first pickled. In the present invention, this pickling is carried out by immersion in an acidic solution containing mainly sulfuric acid, excluding hydrochloric acid. Specifically, as shown in Figure 1, 90% of concentrated sulfuric acid is placed in tank 6.
An acidic solution 7 of ~98 vol% and the remainder of concentrated nitric acid is contained, and the cap 1 is immersed in this acidic solution 7. Further, an ultrasonic oscillation source 8 is attached to a part of the tank 6 to apply ultrasonic vibration to the acidic solution 7. Then,
In the acidic solution 7, the Kovar substrate underlying the oxide film on the exposed surface of the metal shell 2 of the cap 1 was exposed to sulfuric acid.
The oxide film is attacked by H 2 SO 4 and nitric acid HNO 2 and peeled off from its base, and when ultrasonic vibration is applied to this, the oxide film is peeled off and removed from the surface of the metal shell 2. In pickling for the purpose of removing such an oxide film, the low melting point glass 5 of the cap 1 is chemically strong against sulfuric acid and nitric acid, and therefore the phenomenon of elution of the lead component of the low melting point glass 5 hardly occurs. do not have. Although it is not necessarily necessary to apply ultrasonic wave vibration during the above-mentioned pickling, the oxide film on the surface of the metal shell can be removed reliably and at high speed by applying ultrasonic vibration.
次に、酸洗いされたキヤツプ１の金属シエル２
の表面は凹凸面であるので、従来同様にしてキヤ
ツプ１を光沢洗いする。即ち、キヤツプ１を酢酸
溶液84vol％と、硝酸溶液13vol％と、塩酸溶液
1vol％の混合溶液に浸漬して、金属シエル２の表
面を円滑面にする。この光沢洗いで、最初の塩酸
溶液にキヤツプ１を浸漬した時に、低融点ガラス
５の鉛成分が塩酸と反応して溶出することが考え
られるが、この時の塩酸溶液は塩酸濃度が１％と
極薄いものであるので問題無い。また、光沢洗い
されたキヤツプ１の金属シエル２の表面の水との
親和性を良くするために、光沢洗いの後で、キヤ
ツプ１を５〜10％濃度の硫酸溶液、又は５〜10％
濃度の硫酸と硝酸の混合液で軽く洗浄することが
望ましい。 Next, the metal shell 2 of the pickled cap 1
Since the surface of the cap 1 is uneven, the cap 1 is polished in the same manner as before. That is, Cap 1 was mixed with 84 vol% acetic acid solution, 13 vol% nitric acid solution, and hydrochloric acid solution.
The surface of the metal shell 2 is made smooth by immersing it in a 1 vol% mixed solution. When the cap 1 is first immersed in the hydrochloric acid solution during this polishing process, the lead component of the low melting point glass 5 may react with the hydrochloric acid and be eluted, but the hydrochloric acid solution at this time has a hydrochloric acid concentration of 1%. There is no problem since it is extremely thin. In addition, in order to improve the affinity of the surface of the metal shell 2 of the gloss-washed cap 1 with water, after the gloss-washing, the cap 1 is treated with a 5-10% sulfuric acid solution or a 5-10% sulfuric acid solution.
It is recommended to lightly clean with a mixture of concentrated sulfuric acid and nitric acid.
次に、キヤツプ１に、本発明は次のように仕上
げメツキを施す。第２図に示すように、槽９内の
例えば無電解ニツケルメツキ液１０内にキヤツプ
１と、炭素やチタンなどの不溶性電極１１を浸漬
すると共に、直流電源１２で電極１１にプラス電
圧を、キヤツプ１の金属シエル２にマイナス電圧
を印加する。この印加電圧は１〜6V程度のもの
でよい。すると、無電解ニツケルメツキ液１０の
ニツケルの化学的還元に、上述印加電圧により生
じる電気的還元が加わつて、金属シエル２の表面
に付き、仕上げメツキが進行する。この仕上げメ
ツキの場合、金属シエル２の表面に電気的還元に
よるニツケルが速やかにメツキされて、その後に
電気的還元と化学的還元によるメツキが進み、特
に始めの電気的還元によるメツキは、低融点ガラ
ス５から溶出したメツキ液１０との反応生成物が
金属シエル２の表面に流れてくるまでよりも速く
行われる。従つて、低融点ガラス５から溶出した
反応生成物が金属シエル２の表面に達しても、こ
の表面には既にニツケルメツキ層が形成されてい
るので、金属シエル２の表面でのメツキは上述反
応生成物に影響されること無く進行する。 Next, the present invention applies finish plating to the cap 1 as follows. As shown in FIG. 2, the cap 1 and an insoluble electrode 11 made of carbon, titanium, or the like are immersed in, for example, an electroless nickel plating solution 10 in a tank 9, and a positive voltage is applied to the electrode 11 using a DC power source 12. A negative voltage is applied to the metal shell 2. This applied voltage may be about 1 to 6V. Then, the electrical reduction caused by the above-mentioned applied voltage is added to the chemical reduction of nickel in the electroless nickel plating solution 10, and the nickel is attached to the surface of the metal shell 2, and finish plating progresses. In the case of this finishing plating, nickel is quickly plated on the surface of the metal shell 2 by electrical reduction, followed by plating by electrical reduction and chemical reduction. This is done faster than the reaction product with the plating liquid 10 eluted from the glass 5 flows onto the surface of the metal shell 2. Therefore, even if the reaction product eluted from the low melting point glass 5 reaches the surface of the metal shell 2, a nickel plating layer has already been formed on this surface, so the plating on the surface of the metal shell 2 is due to the reaction product mentioned above. Proceed without being influenced by things.
また、本発明における仕上げメツキは化学的還
元と電気的還元の２つの還元作用で行うために、
金属シエル２の表面に所定の厚さでニツケルメツ
キ層を形成するに要する時間が少なくて済む。例
えば、金属シエル２の表面にニツケルメツキ層を
５〜7μｍの厚さで形成する場合、無電解ニツケ
ルメツキだけでは約25〜30分の時間を要していた
のに対し、上記本発明方法においては10〜15分の
時間で済み、この時間の短縮された分だけ低融点
ガラス５からの鉛成分の溶出量が少なくなり、よ
り良好な仕上げメツキが可能となる。 In addition, since finish plating in the present invention is performed by two reduction actions, chemical reduction and electrical reduction,
It takes less time to form a nickel plating layer with a predetermined thickness on the surface of the metal shell 2. For example, when forming a nickel plating layer with a thickness of 5 to 7 μm on the surface of the metal shell 2, it would take about 25 to 30 minutes using electroless nickel plating alone, whereas the method of the present invention described above would take about 10 minutes. The time required is ~15 minutes, and the amount of lead component eluted from the low melting point glass 5 is reduced by the amount of time shortened, and better finish plating is possible.
発明の効果
本発明によれば、金属シエルにガラス板を低融
点ガラスで接着固定したキヤツプの仕上げメツキ
を、低融点ガラスからの酸との反応生成物の溶出
による影響を受けること無く行えて、仕上げメツ
キの均一で良質なキヤツプ製造が可能となる。ま
た、金属シエルの表面に酸化膜を形成しておい
て、金属シエルにガラス板を低融点ガラスで接着
固定する製法が採用でき、気密性に優れたキヤツ
プが提供できる。Effects of the Invention According to the present invention, finish plating of a cap in which a glass plate is adhesively fixed to a metal shell with low melting point glass can be performed without being affected by the elution of reaction products with acid from the low melting point glass. It is possible to manufacture high-quality caps with uniform finish plating. Furthermore, a manufacturing method can be adopted in which an oxide film is formed on the surface of the metal shell and a glass plate is adhesively fixed to the metal shell using low melting point glass, thereby providing a cap with excellent airtightness.
第１図及び第２図は本発明方法を説明するため
のキヤツプ酸洗い装置及びキヤツプ仕上げメツキ
装置の概略側断面図である。第３図は光素子用キ
ヤツプの一例を示す平面図、第４図は第３図のＡ
−Ａ線に沿う断面図である。
１……キヤツプ、２……金属シエル、３……窓
孔、４……ガラス板、５……低融点ガラス。
1 and 2 are schematic side sectional views of a cap pickling device and a cap finishing plating device for explaining the method of the present invention. Figure 3 is a plan view showing an example of a cap for optical elements, and Figure 4 is A of Figure 3.
- It is a sectional view along the A line. 1...Cap, 2...Metal shell, 3...Window hole, 4...Glass plate, 5...Low melting point glass.
Claims (1)
ガラスで接着固定したキヤツプを、塩酸を除く、
硫酸を主体とする酸性溶液で酸洗いする工程と、 酸洗いされた前記キヤツプを無電解金属メツキ
液に浸漬し、キヤツプの金属シエルに電圧を印加
して金属シエル表面を仕上げメツキする工程とを
含むことを特徴とする光素子用キヤツプの製造方
法。[Claims] 1. A cap in which a glass plate is adhesively fixed to the periphery of a window hole of a metal shell with low melting point glass is removed from hydrochloric acid.
A step of pickling with an acidic solution mainly containing sulfuric acid, and a step of immersing the pickled cap in an electroless metal plating solution and applying a voltage to the metal shell of the cap to finish plating the surface of the metal shell. 1. A method of manufacturing a cap for an optical device, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14187786A JPS62298140A (en) | 1986-06-18 | 1986-06-18 | Manufacture of cap for optical element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14187786A JPS62298140A (en) | 1986-06-18 | 1986-06-18 | Manufacture of cap for optical element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62298140A JPS62298140A (en) | 1987-12-25 |
| JPH0376024B2 true JPH0376024B2 (en) | 1991-12-04 |
Family
ID=15302241
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14187786A Granted JPS62298140A (en) | 1986-06-18 | 1986-06-18 | Manufacture of cap for optical element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62298140A (en) |
-
1986
- 1986-06-18 JP JP14187786A patent/JPS62298140A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62298140A (en) | 1987-12-25 |
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